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

HRID 1642485ノート

反応式

HRID 1642485 の反応式
[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

参加物

4

反応物 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

生成物 1

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

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒2 回

実験手順

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.

後処理

  1. customThen solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-346797aef65d49b8a8d143497c2c8554
出典データセット
uspto-grants-2012_02
特許番号
US08119661B2

反応ノート

読み込み中…