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

Formaldehyde → 3-(4-Benzyloxy-3-trifluoromethylbenzoyl)-2,3-dihydro-1,3-benzothiazole

HRID 385116
ノート
印刷プレビュー

反応式

HRID 385116 の反応式
[S:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[NH:3][CH2:2]1.NC1C=CC=CC=1S.C=O.[CH2:20]([O:27][C:28]1[CH:36]=[CH:35][C:31]([C:32](Cl)=[O:33])=[CH:30][C:29]=1[C:37]([F:40])([F:39])[F:38])[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1>C(Cl)(Cl)Cl.C(N(CC)CC)C>[CH2:20]([O:27][C:28]1[CH:36]=[CH:35][C:31]([C:32]([N:3]2[C:4]3[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=3[S:1][CH2:2]2)=[O:33])=[CH:30][C:29]=1[C:37]([F:38])([F:39])[F:40])[C:21]1[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=1
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 4

HCID 712FormaldehydeHCID 87132-AminothiophenolHCID 96588BenzothiazolineHCID 866681754-Benzyloxy-3-trifluoromethylbenzoyl chloride

生成物 1

HCID 681089763-(4-Benzyloxy-3-trifluoromethylbenzoyl)-2,3-dihydro-1,3-benzothiazole

試薬・触媒・溶媒 2

HCID 6212Chloroform
溶媒
HCID 8471Triethylamine溶媒

実験手順

2,3-dihydro-1,3-benzothiazole synthesized from 2-aminobenzenethiol (282 mg) and 37% formalin (0.19 mL) in the same manner as in Example 1 was dissolved in chloroform (6 mL), and triethylamine (0.62 mL) and 4-benzyloxy-3-trifluoromethylbenzoyl chloride were added to the solution, and then the mixture was stirred at mom temperature for 1.5 hours. The solvent was distilled off under reduced pressure and water was added, and then the mixture was extracted with ethyl acetate. The organic layer was washed with 1N hydrochloric acid, 1N sodium hydroxide and saturated brine, and then dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure and the obtained residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=4:1) to obtain the title compound (356 mg) as a pale yellow oily substance.

後処理

  1. distillationThe solvent was distilled off under reduced pressure and water
  2. additionwas added
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe organic layer was washed with 1N hydrochloric acid, 1N sodium hydroxide and saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationThe solvent was distilled off under reduced pressure
  7. customthe obtained residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=4:1)

出典と根拠

ORDレコード
ord-20241d3e0d9f4098ac481fe66ad2b1ea
出典データセット
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08367843B2

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