Water → HCID 21430629、化合物

HRID 437253ノート

反応式

HRID 437253 の反応式
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

参加物

6

反応物 4

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

生成物 1

HCID 21430629HCID 21430629、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-78223a9652c548f59d9f873f7c9e218c
出典データセット
uspto-grants-1977_06
特許番号
US04029801

反応ノート

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