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Dicyclohexylcarbodiimide → HCID 17912566、化合物

HRID 1077705
ノート
印刷プレビュー

反応式

HRID 1077705 の反応式
C1(N=C=NC2CCCCC2)CCCCC1.[F:16][C:17]([F:25])=[CH:18][CH2:19][CH2:20][CH2:21][C:22]([OH:24])=O.[C:26]1([S:32][C:33]2[CH:39]=[CH:38][C:36]([NH2:37])=[CH:35][CH:34]=2)[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1>ClCCl>[C:26]1([S:32][C:33]2[CH:39]=[CH:38][C:36]([NH:37][C:22](=[O:24])[CH2:21][CH2:20][CH2:19][CH:18]=[C:17]([F:16])[F:25])=[CH:35][CH:34]=2)[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=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 10868DicyclohexylcarbodiimideHCID 960814-(Phenylthio)anilineHCID 112980566,6-difluorohex-5-enoic Acid

生成物 1

HCID 17912566HCID 17912566、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

At from 0° to 10°, 20.6 g of N,N'-dicyclohexylcarbodiimide are added, while stirring, in portions to 15 g of 6,6-difluorohex-5-enoic acid in 150 ml of dichloromethane. The mixture is stirred for a further 15 minutes under cooling and then 20.1 g of 4-phenylthioaniline are added in portions. The reaction mixture is stirred for 3 hours at room temperature and then filtered. The organic phase is washed with saturated sodium hydrogen carbonate solution and then dried over sodium sulfate. After concentration by evaporation, the residue is recrystallised from toluene/hexane, yielding the title compound having a melting point of from 80° to 81° (compound no. 2-1).

後処理

  1. temperatureunder cooling
  2. stirringThe reaction mixture is stirred for 3 hours at room temperature
  3. filtrationfiltered
  4. washThe organic phase is washed with saturated sodium hydrogen carbonate solution
  5. dry with materialdried over sodium sulfate
  6. concentrationAfter concentration
  7. customby evaporation
  8. customthe residue is recrystallised from toluene/hexane

出典と根拠

ORDレコード
ord-81c92bff5eef4586a55225460e47036f
出典データセット
uspto-grants-1996_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05545630

反応ノート

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