Hydrochloric Acid → (3S)-3-amino-6-phenyl-2,3-dihydro-1,5-benzoxazepin-4(5H)-one hydrochloride

HRID 1670437노트

반응식

HRID 1670437 반응식
[ClH:1].[O:2]=[C:3]1[NH:9][C:8]2[C:10]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)=[CH:11][CH:12]=[CH:13][C:7]=2[O:6][CH2:5][C@@H:4]1[NH:20]C(=O)OC(C)(C)C.C(OC(C)C)(C)C>O1CCOCC1>[ClH:1].[NH2:20][C@@H:4]1[C:3](=[O:2])[NH:9][C:8]2[C:10]([C:14]3[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=3)=[CH:11][CH:12]=[CH:13][C:7]=2[O:6][CH2:5]1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 7914Diisopropyl EtherHCID 86628749tert-butyl [(3S)-4-oxo-6-phenyl-2,3,4,5-tetrahydro-1,5-benzoxazepin-3-yl]carbamate

생성물 1

HCID 67328140(3S)-3-amino-6-phenyl-2,3-dihydro-1,5-benzoxazepin-4(5H)-one hydrochloride

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

실험 절차

2 mL of dioxane and 1.8 mL of a solution of hydrochloric acid in dioxane (4M) are added to a 25 mL round-bottomed flask containing 85 mg of 43 (0.24 mmol). The mixture is stirred for 4 h at RT under argon. The dioxane is concentrated, and taken up in 10 mL of isopropyl ether. The solid formed is disintegrated with isopropyl ether. 60 mg of amine 44 (cream-coloured solid) are obtained after filtration in the hydrochloride form.

후처리

  1. concentrationThe dioxane is concentrated
  2. customThe solid formed

출처 및 근거

ORD 기록
ord-c41ff219ff934e8a8e72ccdf6967efcf
출처 데이터셋
uspto-grants-2011_08
특허 번호
US07994161B2

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