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

tert-Butyl mercaptan → (5-{4-tert-Butylsulfanyl-2-[(N-cyclopropanecarbonyl-N-ethyl-amino)-methyl]-phenyl}-pyridin-3-yl)-acetic acid

HRID 554639
ノート
印刷プレビュー

反応式

HRID 554639 の反応式
[H-].[Na+].[CH3:3][C:4]([SH:7])([CH3:6])[CH3:5].C([O:10][C:11](=[O:35])[CH2:12][C:13]1[CH:14]=[N:15][CH:16]=[C:17]([C:19]2[CH:24]=[CH:23][C:22](F)=[CH:21][C:20]=2[CH2:26][N:27]([C:30]([CH:32]2[CH2:34][CH2:33]2)=[O:31])[CH2:28][CH3:29])[CH:18]=1)C>CN(C=O)C.O.N#N>[C:4]([S:7][C:22]1[CH:23]=[CH:24][C:19]([C:17]2[CH:18]=[C:13]([CH2:12][C:11]([OH:35])=[O:10])[CH:14]=[N:15][CH:16]=2)=[C:20]([CH2:26][N:27]([C:30]([CH:32]2[CH2:34][CH2:33]2)=[O:31])[CH2:28][CH3:29])[CH:21]=1)([CH3:6])([CH3:5])[CH3:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 6387tert-Butyl mercaptanHCID 24758Sodium hydrideHCID 58565012(5-{2-[(N-Cyclopropanecarbonyl-N-ethyl-amino)-methyl]-4fluoro-phenyl}-pyridin-3-yl)-acetic acid ethyl ester

生成物 1

HCID 45138778(5-{4-tert-Butylsulfanyl-2-[(N-cyclopropanecarbonyl-N-ethyl-amino)-methyl]-phenyl}-pyridin-3-yl)-acetic acid

試薬・触媒・溶媒 3

HCID 947Nitrogen溶媒
HCID 962Water溶媒
HCID 6228Dimethylformamide溶媒

実験手順

Sodium hydride (60% in mineral oil; 0.042 g, 1.04 mmol) was suspended in DMF (5 mL). After stirring for 10 minutes, 2-methyl-2-propanethiol (0.13 mL, 1.15 mmol) was added, and the mixture was stirred for 30 minutes. (5-{2-[(N-Cyclopropanecarbonyl-N-ethyl-amino)-methyl]-4-fluoro-phenyl}-pyridin-3-yl)-acetic acid ethyl ester (0.20 g, 0.52 mmol) was added, and the reaction was stirred at 90° C. overnight. The mixture was diluted with H2O, and N2 was bubbled through the solution into a bleach trap until all odor was removed. The aqueous layer was washed with EtOAc, and then acidified to pH 4 and extracted with EtOAc. The combined organic layers were concentrated, and the residue was purified by preparative HPLC to give Compound 22.

後処理

  1. stirringthe mixture was stirred for 30 minutes
  2. stirringthe reaction was stirred at 90° C. overnight
  3. customwas bubbled through the solution into a bleach trap until all odor
  4. customwas removed
  5. washThe aqueous layer was washed with EtOAc
  6. extractionextracted with EtOAc
  7. concentrationThe combined organic layers were concentrated
  8. customthe residue was purified by preparative HPLC

出典と根拠

ORDレコード
ord-d857485f4ea04e04a8c56b161bd5d003
出典データセット
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08049015B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート