Sodium Hydroxide → HCID 13478355, 화합물

HRID 371474노트

반응식

HRID 371474 반응식
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

참가 물질

4

반응물 2

HCID 14798Sodium Hydroxide2회HCID 13478346HCID 13478346, 화합물

생성물 1

HCID 13478355HCID 13478355, 화합물

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-4d514cacd1fa44b4a7d0a4c9d8b523fc
출처 데이터셋
uspto-grants-1985_07
특허 번호
US04532240

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