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

Trifluoroacetic acid → HCID 178489242、化合物

HRID 2040107
ノート
印刷プレビュー

反応式

HRID 2040107 の反応式
C(OC([N:8]1[CH2:13][CH2:12][O:11][CH:10]([CH2:14][NH:15][C:16]2[S:17][C:18](=[CH:22][C:23]3[CH:28]=[CH:27][C:26]([O:29][C:30]4[CH:35]=[CH:34][C:33]([C:36]#[N:37])=[CH:32][C:31]=4[C:38]([F:41])([F:40])[F:39])=[C:25]([O:42][CH3:43])[CH:24]=3)[C:19](=[O:21])[N:20]=2)[CH2:9]1)=O)(C)(C)C.FC(F)(F)C(O)=O>ClCCl>[CH3:43][O:42][C:25]1[CH:24]=[C:23]([CH:22]=[C:18]2[S:17][C:16]([NH:15][CH2:14][CH:10]3[O:11][CH2:12][CH2:13][NH:8][CH2:9]3)=[N:20][C:19]2=[O:21])[CH:28]=[CH:27][C:26]=1[O:29][C:30]1[CH:35]=[CH:34][C:33]([C:36]#[N:37])=[CH:32][C:31]=1[C:38]([F:40])([F:39])[F:41]
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

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 178489243HCID 178489243、化合物

生成物 1

HCID 178489242HCID 178489242、化合物収率 63%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

LC/MS (m/z) [M+1]+618.8 (calculated for C29H29F3N4O6S, 618.63). 2-({5-[4-(4-Cyano-2-trifluoromethyl-phenoxy)-3-methoxy-benzylidene]-4-oxo-4,5-dihydro-thiazol-2-ylamino}-methyl)-morpholine-4-carboxylic acid tert-butyl ester (0.1 g, 0.16 mmol) was dissolved in dry dichloromethane (6 mL). To the reaction mixture was then added at 0° C. trifluoroacetic acid (2 mL). The reaction mixture was stirred at 0° C. for 1 hour and then at room temperature for 30 minutes. The reaction mixture was then partitioned with saturated aqueous sodium bicarbonate and dichloromethane. The organic layer was washed with brine, dried with Na2SO4, filtered and the solvent evaporated in vacuo to yield a crude oil. The crude oil was purified via flash chromatography (6% ammonia 2.0 M methanol/dichloromethane) to yield the compound as a solid (0.052 g, 63%).

後処理

  1. waitat room temperature for 30 minutes
  2. customThe reaction mixture was then partitioned with saturated aqueous sodium bicarbonate and dichloromethane
  3. washThe organic layer was washed with brine
  4. dry with materialdried with Na2SO4
  5. filtrationfiltered
  6. customthe solvent evaporated in vacuo
  7. customto yield a crude oil
  8. customThe crude oil was purified via flash chromatography (6% ammonia 2.0 M methanol/dichloromethane)

出典と根拠

ORDレコード
ord-923a3678257240689c14a56cf8bc160f
出典データセット
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08580832B2

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