Dimethylcarbamoyl Chloride → HCID 178484724, 화합물

HRID 16120

반응식

HRID 16120 반응식
Cl.Cl.Cl.[Cl:4][C:5]1[C:10]([Cl:11])=[CH:9][CH:8]=[CH:7][C:6]=1[N:12]1[CH2:17][CH2:16][N:15]([CH2:18][CH2:19][C@H:20]2[CH2:25][CH2:24][C@H:23]([NH2:26])[CH2:22][CH2:21]2)[CH2:14][CH2:13]1.C(N(CC)CC)C.[CH3:34][N:35]([CH3:39])[C:36](Cl)=[O:37]>ClCCl>[Cl:4][C:5]1[C:10]([Cl:11])=[CH:9][CH:8]=[CH:7][C:6]=1[N:12]1[CH2:17][CH2:16][N:15]([CH2:18][CH2:19][C@H:20]2[CH2:25][CH2:24][C@H:23]([NH:26][C:36]([N:35]([CH3:39])[CH3:34])=[O:37])[CH2:22][CH2:21]2)[CH2:14][CH2:13]1

참가 물질

5

반응물 3

HCID 6598Dimethylcarbamoyl ChlorideHCID 8471TriethylamineHCID 178478588HCID 178478588, 화합물

생성물 1

HCID 178484724HCID 178484724, 화합물수율 65%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

1.39 g (3 mmol) trans-4-{2-[4-(2,3-dichlorophenyl)-piperazin-1-yl]-ethyl}-cyclohexyl-amine trihydrochloride was suspended in dichloromethane (100 ml), triethylamine (2.1 ml, 15 mmol) was added followed by 0.30 ml (3.3 mmol) N,N-dimethylcarbamoylchloride. The reaction mixture was stirred for 48 hours at room temperature, filtered. The filtrate was washed with water (2×20 ml), dried and evaporated in vacuo. Recrystallizing from methanol gave the title compound (0.83 g, 65%), melting at 212-4° C.

후처리

  1. filtrationfiltered
  2. washThe filtrate was washed with water (2×20 ml)
  3. customdried
  4. customevaporated in vacuo
  5. customRecrystallizing from methanol

출처 및 근거

ORD 기록
ord-6738cef98f8145c9991bc3321e90ddd0
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07737142B2

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