4-Chlorobenzenesulfonyl chloride → HCID 18697990, 화합물

HRID 2289544노트

반응식

HRID 2289544 반응식
C(OC([N:8]1[CH2:13][CH2:12][N:11]([C:14]([N:16]2[CH2:21][CH2:20][N:19]([C:22]3[CH:27]=[CH:26][N:25]=[C:24]([CH3:28])[N:23]=3)[CH2:18][CH2:17]2)=[O:15])[CH2:10][CH2:9]1)=O)(C)(C)C.C(N(CC)CC)C.[Cl:36][C:37]1[CH:42]=[CH:41][C:40]([S:43](Cl)(=[O:45])=[O:44])=[CH:39][CH:38]=1>ClCCl>[Cl:36][C:37]1[CH:42]=[CH:41][C:40]([S:43]([N:8]2[CH2:13][CH2:12][N:11]([C:14]([N:16]3[CH2:21][CH2:20][N:19]([C:22]4[CH:27]=[CH:26][N:25]=[C:24]([CH3:28])[N:23]=4)[CH2:18][CH2:17]3)=[O:15])[CH2:10][CH2:9]2)(=[O:45])=[O:44])=[CH:39][CH:38]=1

참가 물질

5

반응물 3

HCID 73984-Chlorobenzenesulfonyl chlorideHCID 8471TriethylamineHCID 18697989HCID 18697989, 화합물

생성물 1

HCID 18697990HCID 18697990, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

1-(tert-butoxycarbonyl)-4-(1-(2-methylpyrimidin-4-yl)piperazin-4-ylcarbonyl)piperazine (700 mg) was stirred in dichloromethane (20 ml) and triethylarnine (1.34 ml) and cooled in an ice-bath. 4-chlorobenzenesulphonylchloride (0.56 g) was added and reaction allowed to warm to room temperature and then stirred overnight. The mixture was evaporated and the residue was purified by chromatography on silica gel using in gradient of dichloromethane to 8% methanol in dichloromethane as eluent to give a foam. This was triturated with diethylether to give 1-(4-chlorophenylsulphonyl)-4-[1-(2-methylpyrimidin-4-yl)piperazin-4-ylcarbonyl]piperazine a colourless solid 1.05 g ;m.p. 183-184° C.; NMR (CDCl3): 8.15 (m, 1H), 7.7 (m, 2H), 7.55 (m, 2H), 6.3 (m, 1H), 3.65 (m, 4H), 3.45 (m, 4H), 3.35 (m, 4H), 3.05 (m, 4H), 2.5 (s, 3H).

후처리

  1. customreaction
  2. customThe mixture was evaporated
  3. customthe residue was purified by chromatography on silica gel using in gradient of dichloromethane to 8% methanol in dichloromethane as eluent
  4. customto give a foam
  5. customThis was triturated with diethylether

출처 및 근거

ORD 기록
ord-8b4ff46da9a74baf9bde49c438fbbfa0
출처 데이터셋
uspto-grants-2000_07
특허 번호
US06093718

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