Dicyclohexylcarbodiimide → HCID 178442095、化合物

HRID 1198327

反応式

HRID 1198327 の反応式
C1(N=C=NC2CCCCC2)CCCCC1.[CH2:16]([C:21]1[CH:26]=[CH:25][C:24]([C:27]2[CH:32]=[CH:31][C:30]([OH:33])=[C:29]([F:34])[C:28]=2[F:35])=[CH:23][CH:22]=1)[CH2:17][CH2:18][CH2:19][CH3:20].[CH2:36]([C@H:41]1[CH2:46][CH2:45][C@H:44]([C:47](O)=[O:48])[CH2:43][CH2:42]1)[CH2:37][CH2:38][CH2:39][CH3:40]>C(Cl)Cl>[CH2:36]([C@H:41]1[CH2:42][CH2:43][C@H:44]([C:47]([O:33][C:30]2[CH:31]=[CH:32][C:27]([C:24]3[CH:23]=[CH:22][C:21]([CH2:16][CH2:17][CH2:18][CH2:19][CH3:20])=[CH:26][CH:25]=3)=[C:28]([F:35])[C:29]=2[F:34])=[O:48])[CH2:45][CH2:46]1)[CH2:37][CH2:38][CH2:39][CH3:40]

参加物

5

反応物 3

HCID 10868DicyclohexylcarbodiimideHCID 191036434'-Pentyl-2,3-difluorobiphenyl-4-olHCID 178444557HCID 178444557、化合物

生成物 1

HCID 178442095HCID 178442095、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

0.1 mol of dicyclohexylcarbodiimide (DCC) dissolved in CH2Cl2 is added to 0.1 mol of 4'-pentyl-2,3-difluorobiphenyl-4-ol (which can be prepared from 4'-pentyl-2,3-difluoro-4-methoxy-biphenyl by ether cleavage with HBr/glacial acetic acid), 0.1 mol of trans-4-n-pentyl-cyclohexanecarboxylic acid and a catalytic amount of 4-N,N'-dimethylaminopyridine (DMAP) in 300 ml of CH2Cl2 at 0° C., with exclusion of moisture. The mixture is then stirred at room temperature for 12 hours, the dicyclohexylurea which has precipitated is separated off and the product is worked up in the customary manner. The product is purified by crystallization. 4'-Pentyl-2,3-difluorobiphenyl-4-yl trans-4-n-Pentylcyclohexanecarboxylate is obtained, C 44° N 159.1° I.

後処理

  1. customat 0° C.
  2. customthe dicyclohexylurea which has precipitated
  3. customis separated off
  4. customThe product is purified by crystallization

出典と根拠

ORDレコード
ord-408bf51ab9bb414cb99c8b65607d7ea1
出典データセット
uspto-grants-1994_01
特許番号
US05279764

関連ノート

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