Hydrochloric Acid → (3aS,7aS)-1-[1-(3-methylpyrrolidin-3-yl)-4-piperidyl]-3a,4,5,6,7,7a-hexahydro-3H-benzoimidazol-2-one

HRID 1642485노트

반응식

HRID 1642485 반응식
[O:1]=[C:2]1[N:6]([CH:7]2[CH2:12][CH2:11][N:10]([C:13]3([CH3:25])[CH2:17][CH2:16][N:15](C(OC(C)(C)C)=O)[CH2:14]3)[CH2:9][CH2:8]2)[C@H:5]2[CH2:26][CH2:27][CH2:28][CH2:29][C@@H:4]2[NH:3]1.Cl>O1CCOCC1>[CH3:25][C:13]1([N:10]2[CH2:11][CH2:12][CH:7]([N:6]3[C@H:5]4[CH2:26][CH2:27][CH2:28][CH2:29][C@@H:4]4[NH:3][C:2]3=[O:1])[CH2:8][CH2:9]2)[CH2:17][CH2:16][NH:15][CH2:14]1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 57619807Tert-butyl 3-[4-[(3aS,7aS)-2-oxo-3a,4,5,6,7,7a-hexahydro-3H-benzoimidazol-1-yl]-1-piperidyl]-3-methyl-pyrrolidine-1-carboxylate

생성물 1

HCID 57619793(3aS,7aS)-1-[1-(3-methylpyrrolidin-3-yl)-4-piperidyl]-3a,4,5,6,7,7a-hexahydro-3H-benzoimidazol-2-one수율 93.2%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

실험 절차

Tert-butyl 3-[4-[(3aS,7aS)-2-oxo-3a,4,5,6,7,7a-hexahydro-3H-benzoimidazol-1-yl]-1-piperidyl]-3-methyl-pyrrolidine-1-carboxylate (1.85 g, 4.55 mmol) in dioxane was added with 4N HCl solution in dioxane (11.4 mL, 45.5 mmol) and was stirred at room temperature under nitrogen atmosphere overnight. Then solvent was removed under reduced pressure to give the title compound as a white solid (1.3 g), which was used for the subsequent step without further purification. MS (M+1): 307.28.

후처리

  1. customThen solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-346797aef65d49b8a8d143497c2c8554
출처 데이터셋
uspto-grants-2012_02
특허 번호
US08119661B2

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