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反応

Hydrochloric Acid → 1-Methyl-4-(2-phenyl-imidazo[1,2-a]pyrimidin-7-ylcarbamoyl)-1H-pyrazole-3-carboxylic acid

HRID 1958334

印刷プレビュー

反応式

HRID 1958334 の反応式

[OH-].[Na+].C([O:5][C:6]([C:8]1[C:12]([C:13](=[O:30])[NH:14][C:15]2[CH:20]=[CH:19][N:18]3[CH:21]=[C:22]([C:24]4[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=4)[N:23]=[C:17]3[N:16]=2)=[CH:11][N:10]([CH3:31])[N:9]=1)=[O:7])C.O.Cl>C1COCC1.CO>[CH3:31][N:10]1[CH:11]=[C:12]([C:13](=[O:30])[NH:14][C:15]2[CH:20]=[CH:19][N:18]3[CH:21]=[C:22]([C:24]4[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=4)[N:23]=[C:17]3[N:16]=2)[C:8]([C:6]([OH:7])=[O:5])=[N:9]1

参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 313Hydrochloric Acid

HCID 14798Sodium Hydroxide

HCID 673923291-Methyl-4-(2-phenyl-imidazo[1,2-a]pyrimidin-7-ylcarbamoyl)-1H-pyrazole-3-carboxylic acid ethyl ester

生成物 1

HCID 673917831-Methyl-4-(2-phenyl-imidazo[1,2-a]pyrimidin-7-ylcarbamoyl)-1H-pyrazole-3-carboxylic acid収率 45%

試薬・触媒・溶媒 2

HCID 887

Methanol

溶媒

HCID 8028Tetrahydrofuran溶媒

実験手順

NaOH (3N, 1.5 ml) was added to a solution of 1-methyl-4-(2-phenyl-imidazo[1,2-a]pyrimidin-7-ylcarbamoyl)-1H-pyrazole-3-carboxylic acid ethyl ester (390 mg, 1.5 mmol) in a mixture of THF (5 ml) and methanol (5 ml), and the mixture was stirred for 3 h at RT. Water (10 ml) was added, and the mixture was acidified (pH=3) by addition of HCl. The mixture was stirred for 30 min and filtered. The obtained precipitate was washed with a small amount of water, and was dried under vacuum. The thus obtained title compound (240 mg, 45%) was pure enough to be used in the next step. MS (m/e)=363.3 [M+H+].

後処理

stirringThe mixture was stirred for 30 min
filtrationfiltered
washThe obtained precipitate was washed with a small amount of water
customwas dried under vacuum

出典と根拠

ORDレコード: ord-c0c38847da11419cb2d6c55328cbbf0d
出典データセット: uspto-grants-2013_04
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US08410117B2

反応ノート

読み込み中…

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