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

Potassium Carbonate → 4-[3-[6-(3-Acetyl-5-trifluoromethanesulfonyloxy-phenoxy)-hexyl]-2-(2-ethoxycarbonyl-ethyl)-phenoxy]-butyric acid ethyl ester

HRID 417042
ノート
印刷プレビュー

反応式

HRID 417042 の反応式
[C:1]([C:4]1[CH:5]=[C:6]([O:11][S:12]([C:15]([F:18])([F:17])[F:16])(=[O:14])=[O:13])[CH:7]=[C:8]([OH:10])[CH:9]=1)(=[O:3])[CH3:2].C(=O)([O-])[O-].[K+].[K+].[CH2:25]([O:27][C:28](=[O:53])[CH2:29][CH2:30][CH2:31][O:32][C:33]1[CH:38]=[CH:37][CH:36]=[C:35]([CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH2:44]Br)[C:34]=1[CH2:46][CH2:47][C:48]([O:50][CH2:51][CH3:52])=[O:49])[CH3:26]>CC(C)=O.CN(C=O)C>[CH2:25]([O:27][C:28](=[O:53])[CH2:29][CH2:30][CH2:31][O:32][C:33]1[CH:38]=[CH:37][CH:36]=[C:35]([CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH2:44][O:10][C:8]2[CH:7]=[C:6]([O:11][S:12]([C:15]([F:18])([F:16])[F:17])(=[O:14])=[O:13])[CH:5]=[C:4]([C:1](=[O:3])[CH3:2])[CH:9]=2)[C:34]=1[CH2:46][CH2:47][C:48]([O:50][CH2:51][CH3:52])=[O:49])[CH3:26]
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

6

反応物 3

HCID 11430Potassium CarbonateHCID 575864914-[3-(6-Bromo-hexyl)-2-(ethoxycarbonyl-ethyl)-phenoxy]-butyric acid ethyl esterHCID 59833966Trifluoro-methanesulfonic acid 3-acetyl-5-hydroxy-phenyl ester

生成物 1

HCID 594968454-[3-[6-(3-Acetyl-5-trifluoromethanesulfonyloxy-phenoxy)-hexyl]-2-(2-ethoxycarbonyl-ethyl)-phenoxy]-butyric acid ethyl ester収率 72%

試薬・触媒・溶媒 2

HCID 180
Acetone
溶媒
HCID 6228Dimethylformamide溶媒

反応条件

温度
75 °C

実験手順

To a solution of trifluoro-methanesulfonic acid 3-acetyl-5-hydroxy-phenyl ester (1.0 g) in a mixture of acetone and DMF (2:1, 80 mL) were added potassium carbonate (2.4 g) and 4-[3-(6-bromo-hexyl)-2-(2-ethoxycarbonyl-ethyl)-phenoxy]-butyric acid ethyl ester (1.8 g). The resulting mixture was stirred at 75° C. for 3 h. Then the insoluble material was filtered out and the filtrate was diluted with ethyl acetate and washed with water and brine. The organic extract was dried over anhydrous sodium sulfate, concentrated and purified on a silica gel column using ethyl acetate and hexanes to yield 1.7 g of the title compound (72% yield). HRMS calcd for C32H41O10S1F3 [M+H]+ 675.2446, observed 675.2440.

後処理

  1. filtrationThen the insoluble material was filtered out
  2. additionthe filtrate was diluted with ethyl acetate
  3. washwashed with water and brine
  4. extractionThe organic extract
  5. dry with materialwas dried over anhydrous sodium sulfate
  6. concentrationconcentrated
  7. custompurified on a silica gel column

出典と根拠

ORDレコード
ord-16331b2026a24f0cb41dbff6c529271d
出典データセット
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08088936B2

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