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

2-Dimethylaminopyridine → {6-[bis-(4-methoxy-phenyl)-phenyl-methoxy]-2,3,4,5-tetrahydroxy-hexyl}-carbamic acid 9H-fluoren-9-ylmethyl ester

HRID 2075644
ノート
印刷プレビュー

反応式

HRID 2075644 の反応式
[CH:1]1[C:13]2[CH:12]([CH2:14][O:15][C:16](=[O:29])[NH:17][CH2:18][CH:19]([OH:28])[CH:20]([OH:27])[CH:21]([OH:26])[CH:22]([OH:25])[CH2:23][OH:24])[C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][CH:2]=1.[CH3:30][O:31][C:32]1[CH:53]=[CH:52][C:35]([C:36](Cl)([C:45]2[CH:50]=[CH:49][CH:48]=[CH:47][CH:46]=2)[C:37]2[CH:42]=[CH:41][C:40]([O:43][CH3:44])=[CH:39][CH:38]=2)=[CH:34][CH:33]=1.CN(C1C=CC=CN=1)C>N1C=CC=CC=1>[CH:1]1[C:13]2[CH:12]([CH2:14][O:15][C:16](=[O:29])[NH:17][CH2:18][CH:19]([OH:28])[CH:20]([OH:27])[CH:21]([OH:26])[CH:22]([OH:25])[CH2:23][O:24][C:36]([C:35]3[CH:52]=[CH:53][C:32]([O:31][CH3:30])=[CH:33][CH:34]=3)([C:37]3[CH:42]=[CH:41][C:40]([O:43][CH3:44])=[CH:39][CH:38]=3)[C:45]3[CH:46]=[CH:47][CH:48]=[CH:49][CH:50]=3)[C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][CH:2]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 218852-DimethylaminopyridineHCID 968311,1'-(Chlorophenylmethylene)bis(4-methoxybenzene)HCID 23132532(2,3,4,5,6-pentahydroxy-hexyl)-carbamic acid 9H-fluoren-9-ylmethyl ester

生成物 1

HCID 58687725{6-[bis-(4-methoxy-phenyl)-phenyl-methoxy]-2,3,4,5-tetrahydroxy-hexyl}-carbamic acid 9H-fluoren-9-ylmethyl ester収率 57.9%

試薬・触媒・溶媒 1

HCID 1049
Pyridine
溶媒
2 回

実験手順

Compound 35 (5.0 g, 12.4 mmol) was dissolved in 100 ml of pyridine and azeotropically boiled. After this operation was conducted two times, the product was dissolved in 100 ml of dry pyridine and cooled with ice in a nitrogen stream. 4,4′-Dimethoxytrityl chloride (5.0 g, 14.9 mmol) and dimethylaminopyridine (1.5 g, 12.4 mmol) were added, the temperature was gradually increased from under ice cooling to room temperature, and this was followed by stirring at room temperature for 17 hours. After the pyridine was evaporated under reduced pressure, the residue was diluted with 500 ml of ethyl acetate. After water was added, the organic phase was separated, after which the water phase was again extracted with ethyl acetate. The ethyl acetate phase was washed with saturated brine, after which it was dried with anhydrous magnesium sulfate. After concentration under reduced pressure, the concentrate was purified by silica gel column chromatography (CHCl3:MeOH=10:1) to yield the desired compound (Compound 36: 5.06 g) at a percent yield of 57.9%.

後処理

  1. temperaturecooled with ice in a nitrogen stream
  2. customAfter the pyridine was evaporated under reduced pressure
  3. additionthe residue was diluted with 500 ml of ethyl acetate
  4. additionAfter water was added
  5. customthe organic phase was separated
  6. extractionafter which the water phase was again extracted with ethyl acetate
  7. washThe ethyl acetate phase was washed with saturated brine
  8. dry with materialafter which it was dried with anhydrous magnesium sulfate
  9. concentrationAfter concentration under reduced pressure
  10. customthe concentrate was purified by silica gel column chromatography (CHCl3:MeOH=10:1)

出典と根拠

ORDレコード
ord-2ad30882265e43eba8d8f36a26a88b24
出典データセット
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07919653B2

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