Water → HCID 67319070, 화합물

HRID 339728

반응식

HRID 339728 반응식
Cl.[Cl:2][C:3]1[CH:4]=[C:5]([N:9]2[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]2)[CH:6]=[CH:7][CH:8]=1.Br[CH2:16][CH2:17][CH2:18][NH:19][C:20](=[O:29])[O:21][CH2:22][C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1.C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[Cl:2][C:3]1[CH:4]=[C:5]([N:9]2[CH2:14][CH2:13][N:12]([CH2:16][CH2:17][CH2:18][NH:19][C:20](=[O:29])[O:21][CH2:22][C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=3)[CH2:11][CH2:10]2)[CH:6]=[CH:7][CH:8]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 256811-(3-Chlorophenyl)piperazine monohydrochlorideHCID 254436Benzyl 3-bromopropylcarbamate

생성물 1

HCID 67319070HCID 67319070, 화합물수율 73.1%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

1-(3-Chlorophenyl)piperazine hydrochloride (5 g, 25.4 mmol), benzyl 3-bromopropylcarbamate (8.3 g, 30.5 mmol) and potassium carbonate (10.5 g, 75.9 mmol) were heated to 80° C. in dimethylformamide (100 ml) for overnight under nitrogen condition. After the reaction complete, the reaction mixture was cooled to room temperature and water was added. The organic layer was extracted with ethyl acetate, and washed with water and brine. After drying with MgSO4, the organic layer was filtered and evaporated under reduced pressure to give the title compound (7.2 g, 73%) as light yellow oil, which was used in the deprotection reaction without further purification.

후처리

  1. extractionThe organic layer was extracted with ethyl acetate
  2. washwashed with water and brine
  3. dry with materialAfter drying with MgSO4
  4. filtrationthe organic layer was filtered
  5. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-e6aa6c02a05147e08425fb3fe3817fda
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08895558B2

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