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

Water → N-(4-Benzoyl-2-methylphenyl)-3,3,3-trifluoro-2-hydroxy-2-methylpropanamide

HRID 374872
ノート
印刷プレビュー

反応式

HRID 374872 の反応式
[F:1][C:2]([F:10])([F:9])[C:3]([OH:8])([CH3:7])[C:4](O)=[O:5].S(Cl)(Cl)=O.[NH2:15][C:16]1[CH:29]=[CH:28][C:19]([C:20]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)=[O:21])=[CH:18][C:17]=1[CH3:30].O>CN(C)C(=O)C.CCCCCC.C(OCC)C.ClCCl>[C:20]([C:19]1[CH:28]=[CH:29][C:16]([NH:15][C:4](=[O:5])[C:3]([OH:8])([CH3:7])[C:2]([F:10])([F:9])[F:1])=[C:17]([CH3:30])[CH:18]=1)(=[O:21])[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 962WaterHCID 21052Benzophenone, 4-amino-3-methyl-HCID 24386Thionyl ChlorideHCID 27751253,3,3-Trifluoro-2-hydroxy-2-methylpropanoic acid

生成物 1

HCID 9819831N-(4-Benzoyl-2-methylphenyl)-3,3,3-trifluoro-2-hydroxy-2-methylpropanamide

試薬・触媒・溶媒 3

HCID 8058Hexane
溶媒
HCID 31374Dimethylacetamide溶媒
HCID 21881112Ethyl ether methylene chloride溶媒

実験手順

To a solution of 3,3,3-trifluoro-2-hydroxy-2-methylpropanoic acid (1.11 g) in N,N-dimethylacetamide (15 mL) at -20° C. was added thionyl chloride (0.84 g) and the mixture was allowed to stir at -10° to -15° C. for 1 hour. 4-Amino-3-methylbenzophenone (1.00 g) was added in one portion and the reaction mixture was stirred at room temperature overnight. The mixture was poured into water and the resultant gummy solid was collected by filtration. The solid was dissolved in methylene chloride, dried and evaporated to give a brown oil. Chromatography, with diethyl ether:dichloromethane (2:98) as the eluent, gave a white foam which was stirred with hexane for two hours. The title compound was collected by filtration as a white solid (1.04 g); mp 123°-124° C.; MS: m/z=352(M+1); NMR: 1.61 (s,3), 2.28 (s,3), 7.54-7.61 (m,3) 7.66-7.74 (m,6) 9.73 (s,1). Analysis for C18H16F3NO3 : Calculated: C, 61.54; H, 4.59; N, 3.99; Found: C, 61.53; H, 4.73; N, 4.01.

後処理

  1. stirringthe reaction mixture was stirred at room temperature overnight
  2. filtrationthe resultant gummy solid was collected by filtration
  3. dissolutionThe solid was dissolved in methylene chloride
  4. customdried
  5. customevaporated
  6. customto give a brown oil
  7. filtrationThe title compound was collected by filtration as a white solid (1.04 g)

出典と根拠

ORDレコード
ord-8a01073b36c24dc79dbb4f0545aeedcb
出典データセット
uspto-grants-1996_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05482969

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