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Dimethylformamide → HCID 18182333、化合物

HRID 1359415
ノート
印刷プレビュー

反応式

HRID 1359415 の反応式
[Br:1]N1C(=O)CCC1=O.CN(C)C=O.[CH2:14]([C:21]1[C:22]2[CH2:29][CH2:28][CH:27]([CH2:30][OH:31])[CH2:26][C:23]=2[S:24][CH:25]=1)[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1>O>[Br:1][C:25]1[S:24][C:23]2[CH2:26][CH:27]([CH2:30][OH:31])[CH2:28][CH2:29][C:22]=2[C:21]=1[CH2:14][C:15]1[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=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 6228DimethylformamideHCID 67184N-bromobutanimideHCID 18182277HCID 18182277、化合物

生成物 1

HCID 18182333HCID 18182333、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

103 mg of N-bromosuccinimide was added little by little to a solution of 5.0 ml of N,N-dimethylformamide containing 136 mg of 3-benzyl-6-(hydroxymethyl)-4,5,6,7-tetrahydrobenzo[b]thiophene under ice-cooling. After stirring for one hour, water was added to the reaction solution and the mixture was extracted with ethyl acetate. The organic phase was washed with water and brine, and the solvent was removed. Then, the residue was subjected to silica gel column chromatography and eluted with hexane and then with hexane/ethyl acetate (2:1), to give 164 mg of the target compound.

後処理

  1. temperaturecooling
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe organic phase was washed with water and brine
  4. customthe solvent was removed
  5. washeluted with hexane

出典と根拠

ORDレコード
ord-be9a5c15e47d4940873b75586d1ef72f
出典データセット
uspto-grants-2003_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06599917B1

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