Hydrochloric Acid → 4-{[6-Cyclopropyl-3-(pyrimidin-5-ylamino)-pyrazine-2-carbonyl]-amino}-2-methyl-2H-pyrazole-3-carboxylic acid

HRID 467769

反応式

HRID 467769 の反応式
C([O:3][C:4]([C:6]1[N:7]([CH3:30])[N:8]=[CH:9][C:10]=1[NH:11][C:12]([C:14]1[C:19]([NH:20][C:21]2[CH:22]=[N:23][CH:24]=[N:25][CH:26]=2)=[N:18][CH:17]=[C:16]([CH:27]2[CH2:29][CH2:28]2)[N:15]=1)=[O:13])=[O:5])C.[OH-].[Na+].Cl>C(O)C.O>[CH:27]1([C:16]2[N:15]=[C:14]([C:12]([NH:11][C:10]3[CH:9]=[N:8][N:7]([CH3:30])[C:6]=3[C:4]([OH:5])=[O:3])=[O:13])[C:19]([NH:20][C:21]3[CH:26]=[N:25][CH:24]=[N:23][CH:22]=3)=[N:18][CH:17]=2)[CH2:29][CH2:28]1

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 700988464-{[6-cyclopropyl-3-(pyrimidin-5-ylamino)-pyrazine-2-carbonyl]-amino}-2-methyl-2H-pyrazole-3-carboxylic acid ethyl ester

生成物 1

HCID 700980734-{[6-Cyclopropyl-3-(pyrimidin-5-ylamino)-pyrazine-2-carbonyl]-amino}-2-methyl-2H-pyrazole-3-carboxylic acid収率 95%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

反応条件

温度
85 °C

実験手順

To a suspension of 4-{[6-cyclopropyl-3-(pyrimidin-5-ylamino)-pyrazine-2-carbonyl]-amino}-2-methyl-2H-pyrazole-3-carboxylic acid ethyl ester (1.13 g, 2.77 mmol) in ethanol (15 ml) and water (12 ml) was added 1N NaOH (3.32 ml) at r.t. under argon atmosphere. The yellow suspension was stirred at 85° C. for 1 h. After cooling down to r.t., the mixture was treated with 1M HCl (3.3 ml) and stirred for 30 min. The product was collected by filtration, washed with water and EtOH, and dried to yield a light yellow solid (1.0 g, 95%).

後処理

  1. temperatureAfter cooling down to r.t.
  2. stirringstirred for 30 min
  3. filtrationThe product was collected by filtration
  4. washwashed with water and EtOH
  5. customdried

出典と根拠

ORDレコード
ord-e15e9bc129d14e1e8597c032c09720b2
出典データセット
uspto-grants-2014_01
特許番号
US08623866B2

関連ノート

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