Sodium Perborate → HCID 59438049, 화합물

HRID 474209노트

반응식

HRID 474209 반응식
B(O[O-])=[O:2].[Na+].[CH3:6][N:7]1[CH:11]=[C:10]([C:12]2[CH:13]=[CH:14][C:15](=[O:40])[N:16]([CH2:18][C:19]3[CH:24]=[CH:23][CH:22]=[C:21]([C:25]4[N:30]=[CH:29][C:28](B5OC(C)(C)C(C)(C)O5)=[CH:27][N:26]=4)[CH:20]=3)[N:17]=2)[CH:9]=[N:8]1>C1COCC1.O>[OH:2][C:28]1[CH:27]=[N:26][C:25]([C:21]2[CH:20]=[C:19]([CH:24]=[CH:23][CH:22]=2)[CH2:18][N:16]2[C:15](=[O:40])[CH:14]=[CH:13][C:12]([C:10]3[CH:9]=[N:8][N:7]([CH3:6])[CH:11]=3)=[N:17]2)=[N:30][CH:29]=1

참가 물질

5

반응물 2

HCID 517072Sodium PerborateHCID 594380506-(1-Methyl-1H-pyrazol-4-yl)-2-[[3-[5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-2-pyrimidinyl]phenyl]methyl]-3(2H)-pyridazinone

생성물 1

HCID 59438049HCID 59438049, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

8.50 g (85.1 mmol) of sodium perborate are added in portions with ice-cooling to a suspension of 13.4 g (28.4 mmol) of 6-(1-methyl-1H-pyrazol-4-yl)-2-{3-[5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyrimidin-2-yl]benzyl}-2H-pyridazin-3-one in 55 ml of THF and 55 ml of water, and the mixture is stirred at room temperature for 2 hours. The reaction mixture is filtered off through kieselguhr with suction. The filtrate is evaporated to about half of the original volume in vacuo and adjusted to a pH of 1 using 2 N hydrochloric acid. The precipitate formed is filtered off with suction, washed with water and dried in vacuo: 2-[3-(5-hydroxypyrimidin-2-yl)benzyl]-6-(1-methyl-1H-pyrazol-4-yl)-2H-pyridazin-3-one as pale-beige crystals; m.p. 239° C.; ESI 361.

후처리

  1. filtrationThe reaction mixture is filtered off through kieselguhr with suction
  2. customThe filtrate is evaporated to about half of the original volume in vacuo
  3. customThe precipitate formed
  4. filtrationis filtered off with suction
  5. washwashed with water
  6. customdried in vacuo

출처 및 근거

ORD 기록
ord-fc59402665964bd6a1992845b4812b92
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08637518B2

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