Hydrochloric Acid → HCID 178484724, 화합물

HRID 16122

반응식

HRID 16122 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.[CH2:27]([N:29]([CH2:32]C)[CH2:30]C)C.ClC(Cl)([O:37]C(=O)OC(Cl)(Cl)Cl)Cl.Cl>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:27]([N:29]([CH3:32])[CH3:30])=[O:37])[CH2:22][CH2:21]2)[CH2:14][CH2:13]1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 8471Triethylamine2회HCID 94429TriphosgeneHCID 178478588HCID 178478588, 화합물

생성물 1

HCID 178484724HCID 178484724, 화합물수율 143.6%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

0.56 g (1.2 mmol) trans-4-{2-[4-(2,3-dichlorophenyl)-piperazin-1-yl]-ethyl}-cyclohexyl-amine trihydrochloride was suspended in dry dichloromethane (50 ml), triethylamine 0.77 ml, 6 mmol) was added and 0.13 g (0.44 mmol) triphosgene dissolved in dichloromethane was dropped in. After one hour stirring at room temperature dimetilamine hydrochloride (0.49 g, 6 mmol) followed by triethylamine (0.84 ml, 6 mmol) was added and the stirring was continued for 20 hours. The mixture was filtered, the filtrate washed with water, dried and evaporated in vacuo. Recrystallizing the product from methanol gave the title compound (0.27 g, 52%). Melting point: 212-4° C.

후처리

  1. additionwas dropped in
  2. additionwas added
  3. filtrationThe mixture was filtered
  4. washthe filtrate washed with water
  5. customdried
  6. customevaporated in vacuo
  7. customRecrystallizing the product from methanol

출처 및 근거

ORD 기록
ord-258c082de91b464ba0230efdebd317cf
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07737142B2

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