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Water → 3'-(2-Dibenzylaminoacetyl)-4'-fluoromethanesulfonanilide

HRID 2379184
ノート
印刷プレビュー

反応式

HRID 2379184 の反応式
Br[CH2:2][C:3]([C:5]1[CH:6]=[C:7]([CH:13]=[CH:14][C:15]=1[F:16])[NH:8][S:9]([CH3:12])(=[O:11])=[O:10])=[O:4].[CH2:17]([NH:24][CH2:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.O>CN(C)C=O>[CH2:25]([N:24]([CH2:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)[CH2:2][C:3]([C:5]1[CH:6]=[C:7]([CH:13]=[CH:14][C:15]=1[F:16])[NH:8][S:9]([CH3:12])(=[O:11])=[O:10])=[O:4])[C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=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 962WaterHCID 7656DibenzylamineHCID 221413933'-(2-Bromoacetyl)-4'-fluoromethanesulfonanilide

生成物 1

HCID 189580893'-(2-Dibenzylaminoacetyl)-4'-fluoromethanesulfonanilide収率 84.8%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

3'-(2-Bromoacetyl)-4'-fluoromethanesulfonanilide (30 g) was dissolved in 200 ml of N,N-dimethylformamide, a solution of 38 g of dibenzylamine in N,N-dimethylformamide was added with ice-cooling and stirring and the mixture was made to react at room temperature for 1 hour. The reaction mixture was added to water followed by extracting with ethyl acetate. The extract was washed with water, dried, the solvent was evaporated therefrom and the residue was crystallized from diisopropyl ether to give 35 g of 3'-(2-dibenzylaminoacetyl)-4'-fluoromethanesulfonanilide. The crystals were made into hydrochloride to give 35 g of crystals, m.p. 185°-188° C.

後処理

  1. temperaturecooling
  2. customto react at room temperature for 1 hour
  3. extractionby extracting with ethyl acetate
  4. washThe extract was washed with water
  5. customdried
  6. customthe solvent was evaporated
  7. customthe residue was crystallized from diisopropyl ether

出典と根拠

ORDレコード
ord-5a963038e9db42a18b8ec211a5c078ab
出典データセット
uspto-grants-1994_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05360822

反応ノート

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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