Dicyclohexylcarbodiimide → HCID 178442095, 화합물

HRID 1198327

반응식

HRID 1198327 반응식
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]

참가 물질

5

반응물 3

HCID 10868DicyclohexylcarbodiimideHCID 191036434'-Pentyl-2,3-difluorobiphenyl-4-olHCID 178444557HCID 178444557, 화합물

생성물 1

HCID 178442095HCID 178442095, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-408bf51ab9bb414cb99c8b65607d7ea1
출처 데이터셋
uspto-grants-1994_01
특허 번호
US05279764

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