Boron tribromide → HCID 68428755、化合物

HRID 2240289ノート

反応式

HRID 2240289 の反応式
B(Br)(Br)Br.C[O:6][C:7]1[CH:12]=[CH:11][C:10]([N:13]2[C:17](=[O:18])[O:16][C:15]([C:19]([CH3:22])([CH3:21])[CH3:20])=[N:14]2)=[CH:9][CH:8]=1>ClCCl>[OH:6][C:7]1[CH:8]=[CH:9][C:10]([N:13]2[C:17](=[O:18])[O:16][C:15]([C:19]([CH3:22])([CH3:21])[CH3:20])=[N:14]2)=[CH:11][CH:12]=1

参加物

4

反応物 2

HCID 25134Boron tribromideHCID 68428133HCID 68428133、化合物

生成物 1

HCID 68428755HCID 68428755、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

3.5 g of boron tribromide are slowly added dropwise, at −60°, to a mixture of 70 ml of dichloromethane and 1.5 g of 1-methoxy-4-(5-oxo-2-tert-butyl-3,4-diaza-1-oxa-cyclopent-2-en-4-yl)-benzene. The reaction mixture is stirred at room temperature for 12 hours and then discharged onto ice/water. The aqueous mixture is extracted with dichloromethane, the extract is washed with water and concentrated and the residue is recrystallised from toluene/pentane, yielding 1-hydroxy-4-(5-oxo-2-tert-butyl-3,4-diaza-1-oxa-cyclopent-2-en-4-yl)-benzene, which melts at from 170° to 172°.

後処理

  1. extractionThe aqueous mixture is extracted with dichloromethane
  2. washthe extract is washed with water
  3. concentrationconcentrated
  4. customthe residue is recrystallised from toluene/pentane

出典と根拠

ORDレコード
ord-51b37236371b45218905024b8fcdf736
出典データセット
uspto-grants-2010_05
特許番号
US07723362B2

反応ノート

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