Sodium Perborate → HCID 59438049、化合物

HRID 474209ノート

反応式

HRID 474209 の反応式
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

参加物

5

反応物 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

生成物 1

HCID 59438049HCID 59438049、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-fc59402665964bd6a1992845b4812b92
出典データセット
uspto-grants-2014_01
特許番号
US08637518B2

反応ノート

読み込み中…