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 642818ノート

反応式

HRID 642818 の反応式
[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

参加物

5

反応物 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

生成物 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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ff1fdb87989442bc99d42a9b8fefddda
出典データセット
uspto-grants-2010_04
特許番号
US07696195B2

反応ノート

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