Lithium Hydroxide → (R)-2-(4-amino-3-methyl-5-nitro-phenyl)-1-carboxy-ethyl 4-(2-oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidine-1-carboxylate

HRID 642818노트

반응식

HRID 642818 반응식
[Li+].[OH-:2].[O:3]=[C:4]1[N:10]([CH:11]2[CH2:16][CH2:15][N:14]([C:17]([O:19][C@@H:20](OC)[C:21](=C=O)[C:22]3[CH:27]=[C:26]([N+:28]([O-:30])=[O:29])[C:25]([NH2:31])=[C:24]([CH3:32])[CH:23]=3)=[O:18])[CH2:13][CH2:12]2)[CH2:9][CH2:8][C:7]2[CH:37]=[CH:38][CH:39]=[CH:40][C:6]=2[NH:5]1.C1[CH2:45][O:44]CC1>O>[O:3]=[C:4]1[N:10]([CH:11]2[CH2:12][CH2:13][N:14]([C:17]([O:19][C@@H:20]([C:45]([OH:44])=[O:2])[CH2:21][C:22]3[CH:27]=[C:26]([N+:28]([O-:30])=[O:29])[C:25]([NH2:31])=[C:24]([CH3:32])[CH:23]=3)=[O:18])[CH2:15][CH2:16]2)[CH2:9][CH2:8][C:7]2[CH:37]=[CH:38][CH:39]=[CH:40][C:6]=2[NH:5]1

참가 물질

5

반응물 3

HCID 3939Lithium HydroxideHCID 8028TetrahydrofuranHCID 86601628(R)-2-(4-amino-3-methyl-5-nitro-phenyl)-1-methoxy-carbonyl-ethyl 4-(2-oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidine-1-carboxylate

생성물 1

HCID 68609726(R)-2-(4-amino-3-methyl-5-nitro-phenyl)-1-carboxy-ethyl 4-(2-oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidine-1-carboxylate

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A solution of 120 mg (5.0 mmol) LiOH in 5 mL water was metered into a solution of 1.0 g (1.8 mmol) (R)-2-(4-amino-3-methyl-5-nitro-phenyl)-1-methoxy-carbonyl-ethyl 4-(2-oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidine-1-carboxylate in 10 mL THF, the reaction solution was stirred for 4 h at RT and then evaporated down i.vac. The residue was combined with 30 mL water, washed with 30 mL diethyl ether, acidified with 4 M HCl while cooling with an ice bath and stirred for 30 min at RT. The precipitate was filtered off, washed with water and dried.

후처리

  1. customevaporated down i.vac
  2. washwashed with 30 mL diethyl ether
  3. temperaturewhile cooling with an ice bath
  4. stirringstirred for 30 min at RT
  5. filtrationThe precipitate was filtered off
  6. washwashed with water
  7. customdried

출처 및 근거

ORD 기록
ord-ff1fdb87989442bc99d42a9b8fefddda
출처 데이터셋
uspto-grants-2010_04
특허 번호
US07696195B2

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