Hydrochloric Acid → 5-Oxo-1-(3-oxo-3,4-dihydro-2H-pyrido[3,2-b][1,4]oxazin-6-yl)pyrrolidin-3-carboxylic acid

HRID 1847008ノート

反応式

HRID 1847008 の反応式
O.[OH-].[Li+].C[O:5][C:6]([CH:8]1[CH2:12][C:11](=[O:13])[N:10]([C:14]2[CH:15]=[CH:16][C:17]3[O:18][CH2:19][C:20](=[O:24])[NH:21][C:22]=3[N:23]=2)[CH2:9]1)=[O:7].Cl>CO>[O:13]=[C:11]1[N:10]([C:14]2[CH:15]=[CH:16][C:17]3[O:18][CH2:19][C:20](=[O:24])[NH:21][C:22]=3[N:23]=2)[CH2:9][CH:8]([C:6]([OH:7])=[O:5])[CH2:12]1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 168937Lithium hydroxide, monohydrateHCID 867249385-Oxo-1-(3-oxo-3,4-dihydro-2H-pyrido[3,2-b][1,4]oxazin-6-yl)pyrrolidin-3-carboxylic acid methyl ester

生成物 1

HCID 867249395-Oxo-1-(3-oxo-3,4-dihydro-2H-pyrido[3,2-b][1,4]oxazin-6-yl)pyrrolidin-3-carboxylic acid収率 87%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

An aqueous solution (0.1 ml) of lithium hydroxide monohydrate (8.62 mg, 0.206 mmol) was added to a solution of 5-oxo-1-(3-oxo-3,4-dihydro-2H-pyrido[3,2-b][1,4]oxazin-6-yl)pyrrolidin-3-carboxylic acid methyl ester (40 mg, 0.137 mmol) in methanol (0.8 ml) and the mixture was stirred overnight at room temperature. The reaction solution was neutralized by adding 1N hydrochloric acid (0.206 ml), methanol was removed under reduced pressure, the obtained residue was triturated with water and the insoluble material was collected by filtration and dried to yield 32.9 mg (87%) of the title compound in the form of a colorless solid.

後処理

  1. customwas removed under reduced pressure
  2. customthe obtained residue was triturated with water
  3. filtrationthe insoluble material was collected by filtration
  4. customdried

出典と根拠

ORDレコード
ord-b55dafb140f34c5badaeed57d2f21ecb
出典データセット
uspto-grants-2015_02
特許番号
US08952010B2

反応ノート

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