Cyclohexylamine → 2-[2-(4-Chloro-phenyl)-2,4,5,6-tetrahydro-cyclopentapyrazol-3-yl]-2,N-dicyclohexyl-acetamide

HRID 889377노트

반응식

HRID 889377 반응식
FC1C(O[C:9](=[O:32])[CH:10]([C:17]2[N:18]([C:25]3[CH:30]=[CH:29][C:28]([Cl:31])=[CH:27][CH:26]=3)[N:19]=[C:20]3[CH2:24][CH2:23][CH2:22][C:21]=23)[CH:11]2[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]2)=C(F)C(F)=C(F)C=1F.[CH:37]1([NH2:43])[CH2:42][CH2:41][CH2:40][CH2:39][CH2:38]1>CN(C=O)C.CN(C1C=CN=CC=1)C>[Cl:31][C:28]1[CH:27]=[CH:26][C:25]([N:18]2[C:17]([CH:10]([CH:11]3[CH2:12][CH2:13][CH2:14][CH2:15][CH2:16]3)[C:9]([NH:43][CH:37]3[CH2:42][CH2:41][CH2:40][CH2:39][CH2:38]3)=[O:32])=[C:21]3[CH2:22][CH2:23][CH2:24][C:20]3=[N:19]2)=[CH:30][CH:29]=1

참가 물질

5

반응물 2

HCID 7965CyclohexylamineHCID 86657983[2-(4-Chloro-phenyl)-2,4,5,6-tetrahydro-cyclopentapyrazol-3-yl]-cyclohexyl-acetic acid pentafluorophenyl ester

생성물 1

HCID 533902542-[2-(4-Chloro-phenyl)-2,4,5,6-tetrahydro-cyclopentapyrazol-3-yl]-2,N-dicyclohexyl-acetamide수율 40%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6228Dimethylformamide용매

실험 절차

To a suspension of [2-(4-chloro-phenyl)-2,4,5,6-tetrahydro-cyclopentapyrazol-3-yl]-cyclohexyl-acetic acid pentafluorophenyl ester (95 mg, 181 umol) in DMF (0.9 ml) was added cyclohexylamine (30 ul, 271 umol; CAS Reg. No. 108-91-8) and DMAP (66 mg, 543 umol) at ambient temperature under an argon atmosphere. The reaction mixture was stirred at ambient temperature for 30 h. The solvent was removed under reduced pressure to give a brown oil which was purified by preparative thin layer chromatography (silica gel, iPrOAc/heptane) to obtain the title compound (32 mg, 75 umol; 40%) as brown oil. MS: m/e=440.3 [M+H+].

후처리

  1. customat ambient temperature
  2. customThe solvent was removed under reduced pressure
  3. customto give a brown oil which
  4. customwas purified by preparative thin layer chromatography (silica gel, iPrOAc/heptane)

출처 및 근거

ORD 기록
ord-17643325fa3e49cfa39541c6f8bfe71f
출처 데이터셋
uspto-grants-2012_08
특허 번호
US08252826B2

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