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1,4-Dioxane hydrochloride → 6-[(4R)-4-{[3-(7-Methoxy-2-oxoquinoxalin-1(2H)-yl)propyl]amino}-2-oxopyrrolidin-1-yl]-2H-1,4-benzoxazin-3(4H)-one hydrochloride monohydrate

HRID 1847031
ノート
印刷プレビュー

反応式

HRID 1847031 の反応式
[CH3:1][O:2][C:3]1[CH:12]=[C:11]2[C:6]([N:7]=[CH:8][C:9](=[O:34])[N:10]2[CH2:13][CH2:14][CH2:15][NH:16][C@H:17]2[CH2:21][N:20]([C:22]3[CH:23]=[CH:24][C:25]4[O:30][CH2:29][C:28](=[O:31])[NH:27][C:26]=4[CH:32]=3)[C:19](=[O:33])[CH2:18]2)=[CH:5][CH:4]=1.[ClH:35].O1CCOCC1>ClCCl.C(O)C>[OH2:2].[ClH:35].[CH3:1][O:2][C:3]1[CH:12]=[C:11]2[C:6]([N:7]=[CH:8][C:9](=[O:34])[N:10]2[CH2:13][CH2:14][CH2:15][NH:16][C@H:17]2[CH2:21][N:20]([C:22]3[CH:23]=[CH:24][C:25]4[O:30][CH2:29][C:28](=[O:31])[NH:27][C:26]=4[CH:32]=3)[C:19](=[O:33])[CH2:18]2)=[CH:5][CH:4]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 204431481,4-Dioxane hydrochlorideHCID 601617766-[(4R)-4-{[3-(7-Methoxy-2-oxoquinoxalin-1(2H)-yl)propyl]amino}-2-oxopyrrolidin-1-yl]-2H-1,4-benzoxazin-3(4H)-one

生成物 1

HCID 867249586-[(4R)-4-{[3-(7-Methoxy-2-oxoquinoxalin-1(2H)-yl)propyl]amino}-2-oxopyrrolidin-1-yl]-2H-1,4-benzoxazin-3(4H)-one hydrochloride monohydrate収率 147.7%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒
HCID 6344
Dichloromethane
溶媒

反応条件

温度
50 °C

実験手順

6-[(4R)-4-{[3-(7-Methoxy-2-oxoquinoxalin-1(2H)-yl)propyl]amino}-2-oxopyrrolidin-1-yl]-2H-1,4-benzoxazin-3(4H)-one (2.86 g, 6.17 mmol) was dissolved in dichloromethane (50 ml) and ethanol (2 ml). To this solution was added 4 N hydrogen chloride/dioxane solution (1.59 ml, 6.37 mmol) under cooling in an ice bath. The precipitated insoluble material was collected by filtration and was then dried. The obtained residue was suspended in ethanol (20 ml), and the suspension was then stirred at 50° C. for 20 minutes. The suspension was cooled in an ice bath, and the insoluble material was collected by filtration. The filtrate was dried at 70° C. overnight under reduced pressure to yield 2.36 g (74%) of the above-captioned compound in the form of a colorless solid.

後処理

  1. temperatureunder cooling in an ice bath
  2. filtrationThe precipitated insoluble material was collected by filtration
  3. customwas then dried
  4. temperatureThe suspension was cooled in an ice bath
  5. filtrationthe insoluble material was collected by filtration
  6. customThe filtrate was dried at 70° C. overnight under reduced pressure

出典と根拠

ORDレコード
ord-bc610aeabd144bb3b3db35a1e5778625
出典データセット
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08952010B2

反応ノート

読み込み中…

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