Sodium Hydroxide → HCID 13478355、化合物

HRID 371474ノート

反応式

HRID 371474 の反応式
C[O:2][C:3](=[O:29])[CH2:4][NH:5][C:6](=[O:28])[C:7]1[CH:12]=[CH:11][C:10]([N:13]2[CH2:18][CH2:17][N:16]([C:19]3[C:20]([NH2:27])=[N:21][C:22]([NH2:26])=[N:23][C:24]=3[CH3:25])[CH2:15][CH2:14]2)=[CH:9][CH:8]=1.[OH-].[Na+]>CO>[NH2:26][C:22]1[N:21]=[C:20]([NH2:27])[C:19]([N:16]2[CH2:15][CH2:14][N:13]([C:10]3[CH:9]=[CH:8][C:7]([C:6]([NH:5][CH2:4][C:3]([OH:29])=[O:2])=[O:28])=[CH:12][CH:11]=3)[CH2:18][CH2:17]2)=[C:24]([CH3:25])[N:23]=1

参加物

4

反応物 2

HCID 14798Sodium Hydroxide2 回HCID 13478346HCID 13478346、化合物

生成物 1

HCID 13478355HCID 13478355、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

A mixture of 1.5 g (3.76 mmole) of N-[4-[4-(2,4-diamino-6-methyl-5-pyrimidinyl)-1-piperazinyl]benzoylglycine methyl ester and 3.8 ml (3.8 mmole of a 1N aqueous sodium hydroxide solution in 500 ml of methanol was stirred at room temperature for 16 hours. The reaction mixture remained cloudy. A solution of 0.4 ml of 1N sodium hydroxide in 200 ml of methanol was added and the reaction mixture was stirred for another two hours and became clear solution. Methanol was removed in vacuo. The solid residue was dissolved in 200 ml of water and filtered. The filtrate was acidified with citric acid to pH 6. The precipitate was collected, washed with water, and triturated with 200 ml of boiling methanol. After drying in vacuo at 78° C. for 16 hours, 1.30 g of the product was obtained as white powder, mp>310° C.

後処理

  1. stirringthe reaction mixture was stirred for another two hours
  2. customMethanol was removed in vacuo
  3. dissolutionThe solid residue was dissolved in 200 ml of water
  4. filtrationfiltered
  5. customThe precipitate was collected
  6. washwashed with water
  7. customtriturated with 200 ml of boiling methanol
  8. customAfter drying in vacuo at 78° C. for 16 hours

出典と根拠

ORDレコード
ord-4d514cacd1fa44b4a7d0a4c9d8b523fc
出典データセット
uspto-grants-1985_07
特許番号
US04532240

反応ノート

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