Water → HCID 21430629, 화합물

HRID 437253노트

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HRID 437253 반응식
Cl.Cl.[NH2:3][CH:4]1[CH2:9][CH2:8][N:7]([CH2:10][CH2:11][CH2:12][C:13]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)=[O:14])[CH2:6][CH2:5]1.O.C(=O)([O-])[O-:23].[K+].[K+].[CH2:28](Cl)[C:29]1[CH:37]=[CH:36][C:35]2[O:34][CH2:33][O:32][C:31]=2[CH:30]=1>C(Cl)(Cl)Cl>[C:28]([NH:3][CH:4]1[CH2:9][CH2:8][N:7]([CH2:10][CH2:11][CH2:12][C:13]([C:15]2[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=2)=[O:14])[CH2:6][CH2:5]1)(=[O:23])[C:29]1[CH:37]=[CH:36][C:35]2[O:34][CH2:33][O:32][C:31]=2[CH:30]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 887131,3-Benzodioxole, 5-(chloromethyl)-HCID 227548374-Amino-1-(4-phenyl-4-oxobutyl)piperidine dihydrochloride

생성물 1

HCID 21430629HCID 21430629, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

4-Amino-1-(4-phenyl-4-oxobutyl)piperidine dihydrochloride (3.19 g.) was stirred in chloroform (50 ml.). Water (20 ml.) containing potassium carbonate (8.28 g.) was added followed by dropwise addition of piperonyl chloride (1.84 g.) in chloroform (10 ml.). The mixture was stirred for 18 hr. Some of the title compound separated as the free base and was filtered off. The two-phase filtrate was separated and the remainder of the title compound (base) obtained. The combined bases were dissolved in ethanol/HCl and ether added until crystallisation occurred. Filtration afforded the title compound as the hydrochloride, three-quarter hydrate, colorless prisms (3.876 g.) m.p. 235.7°.

후처리

  1. additionwas added
  2. customSome of the title compound separated as the free base
  3. filtrationwas filtered off
  4. customThe two-phase filtrate was separated

출처 및 근거

ORD 기록
ord-78223a9652c548f59d9f873f7c9e218c
출처 데이터셋
uspto-grants-1977_06
특허 번호
US04029801

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