ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

1,2-Dimethoxyethane → 1H-Indole-2-propanoic acid, 3-[(1,1-dimethylethyl)thio]-1-[[4-(6-ethoxy-3-pyridinyl)phenyl]methyl]-5-hydroxy-alpha,alpha-dimethyl-, ethyl ester

HRID 1620808
ノート
印刷プレビュー

反応式

HRID 1620808 の反応式
C(COC)OC.[CH2:7]([O:9][C:10](=[O:46])[C:11]([CH3:45])([CH3:44])[CH2:12][C:13]1[N:14]([CH2:28][C:29]2[CH:34]=[CH:33][C:32](B3OC(C)(C)C(C)(C)O3)=[CH:31][CH:30]=2)[C:15]2[C:20]([C:21]=1[S:22][C:23]([CH3:26])([CH3:25])[CH3:24])=[CH:19][C:18]([OH:27])=[CH:17][CH:16]=2)[CH3:8].Br[C:48]1[CH:49]=[CH:50][C:51]([O:54][CH2:55][CH3:56])=[N:52][CH:53]=1.C(=O)([O-])[O-].[K+].[K+]>C(OC)(C)(C)C.O>[CH2:7]([O:9][C:10](=[O:46])[C:11]([CH3:45])([CH3:44])[CH2:12][C:13]1[N:14]([CH2:28][C:29]2[CH:34]=[CH:33][C:32]([C:48]3[CH:53]=[N:52][C:51]([O:54][CH2:55][CH3:56])=[CH:50][CH:49]=3)=[CH:31][CH:30]=2)[C:15]2[C:20]([C:21]=1[S:22][C:23]([CH3:26])([CH3:25])[CH3:24])=[CH:19][C:18]([OH:27])=[CH:17][CH:16]=2)[CH3:8]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 80711,2-DimethoxyethaneHCID 11430Potassium CarbonateHCID 8172375-Bromo-2-ethoxypyridineHCID 44474908Ethyl 3-(3-(tert-butylthio)-5-hydroxy-1-(4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzyl)-1H-indol-2-yl)-2,2-dimethylpropanoate

生成物 1

HCID 579717581H-Indole-2-propanoic acid, 3-[(1,1-dimethylethyl)thio]-1-[[4-(6-ethoxy-3-pyridinyl)phenyl]methyl]-5-hydroxy-alpha,alpha-dimethyl-, ethyl ester
収率 80.2%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 15413tert-Butyl methyl ether溶媒

反応条件

温度
75 °C

実験手順

To a stirring mixture of dimethoxyethane (16.5 L) and water (6.6 L) in a 50 L reaction flask under nitrogen was added 3-{3-tert-butylsulfanyl-5-hydroxy-1-[4-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-benzyl]-1H-indol-2-yl}-2,2-dimethyl-propionic acid ethyl ester (1652.19 g), 5-bromo-2-ethoxypyridine (650.30 g), and potassium carbonate (605.03 g). The mixture was sparged with nitrogen for 30 minutes to remove dissolved oxygen gas, and then tetrakis(triphenylphosphine)palladium(0) (59.15 g) was added, and the reaction mixture was heated to 65-85° C. over 2 hours and stirred at 65-85° C. under nitrogen for 19 hours. Once no starting material was seen by tlc analysis, the reaction was cooled to 40° C. and water (6.6 L) was added. Ethyl acetate (6.6 L) was added, and the mixture was agitated for 20 minutes and then allowed to separate over 1.5 hours. The aqueous layer was separated, and additional water (6.6 L) was added to the organic layer. The mixture was agitated for 2 minutes and then allowed to separate over 1 hour, with additional ethyl acetate (1.4 L) added to facilitate phase separation. The aqueous layer was separated, and the two aqueous layers were combined. Ethyl acetate (5.0 L) was added to the combined aqueous layer, and the mixture was agitated for 3 minutes and allowed to separate over 2 minutes. The aqueous layer was separated, and the two organic layers were combined and treated with activated carbon, Novit Neutral (446.43 g). The mixture was stirred for 17 hours at room temperature, and then filtered through a 1-2″ pad of Celite. The reaction flask was rinsed twice with ethyl acetate (1.25 L) and filtered through the pad of Celite, and the filtrate was concentrated to give the crude material. Methyl tert-butyl ether (8.2 L) was added to the solids, and the mixture was agitated for 1.5 hours and filtered. The flask was rinsed with methyl tert-butyl ether (1 L) three times and then filtered through the filter cake. The isolated solids were dried in a drying oven at 25° C. under vacuum for 3 days to give the desired product (1314 g).

後処理

  1. customin a 50 L reaction flask under nitrogen
  2. customThe mixture was sparged with nitrogen for 30 minutes
  3. customto remove
  4. dissolutiondissolved oxygen gas
  5. additiontetrakis(triphenylphosphine)palladium(0) (59.15 g) was added
  6. temperaturethe reaction was cooled to 40° C.
  7. additionwater (6.6 L) was added
  8. additionEthyl acetate (6.6 L) was added
  9. stirringthe mixture was agitated for 20 minutes
  10. customto separate over 1.5 hours
  11. customThe aqueous layer was separated
  12. additionadditional water (6.6 L) was added to the organic layer
  13. stirringThe mixture was agitated for 2 minutes
  14. customto separate over 1 hour, with additional ethyl acetate (1.4 L)
  15. additionadded
  16. customphase separation
  17. customThe aqueous layer was separated
  18. additionEthyl acetate (5.0 L) was added to the combined aqueous layer
  19. stirringthe mixture was agitated for 3 minutes
  20. customto separate over 2 minutes
  21. customThe aqueous layer was separated
  22. additiontreated with activated carbon, Novit Neutral (446.43 g)
  23. stirringThe mixture was stirred for 17 hours at room temperature
  24. filtrationfiltered through a 1-2″ pad of Celite
  25. washThe reaction flask was rinsed twice with ethyl acetate (1.25 L)
  26. filtrationfiltered through the pad of Celite
  27. concentrationthe filtrate was concentrated
  28. customto give the crude material
  29. stirringthe mixture was agitated for 1.5 hours
  30. filtrationfiltered
  31. washThe flask was rinsed with methyl tert-butyl ether (1 L) three times
  32. filtrationfiltered through the filter cake
  33. customThe isolated solids were dried in a drying oven at 25° C. under vacuum for 3 days

出典と根拠

ORDレコード
ord-0e3ac11abb274237aeed3b42f9172af0
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08772495B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート