Boron tribromide → 8-Hydroxy-1,3,4,5-tetrahydrobenzo[b]azepin-2-one

HRID 490696ノート

反応式

HRID 490696 の反応式
C[O:2][C:3]1[CH:4]=[CH:5][C:6]2[CH2:12][CH2:11][CH2:10][C:9](=[O:13])[NH:8][C:7]=2[CH:14]=1.B(Br)(Br)Br>C(Cl)Cl>[OH:2][C:3]1[CH:4]=[CH:5][C:6]2[CH2:12][CH2:11][CH2:10][C:9](=[O:13])[NH:8][C:7]=2[CH:14]=1

参加物

4

反応物 2

HCID 25134Boron tribromideHCID 6769538-methoxy-2,3,4,5-tetrahydro-1H-1-benzazepin-2-one

生成物 1

HCID 99205198-Hydroxy-1,3,4,5-tetrahydrobenzo[b]azepin-2-one収率 89%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of 8-methoxy-1,3,4,5-tetrahydro-benzo[b]azepin-2-one (116 mg, 0.607 mmol) in CH2Cl2 (20 mL) at 0° C. is treated with BBr3 (1.2 mL, 1.0 M in CH2Cl2) added dropwise. The mixture is stirred for 16 hours at room temperature and then quenched with water dropwise. The suspension is filtered and the solid is rinsed with MeOH (1.0 mL) and dried under vacuum to obtain pure product (95 mg, 89%).

後処理

  1. additionadded dropwise
  2. customquenched with water dropwise
  3. filtrationThe suspension is filtered
  4. washthe solid is rinsed with MeOH (1.0 mL)
  5. customdried under vacuum

出典と根拠

ORDレコード
ord-1f73fba40ba5460aafd874fbeba60480
出典データセット
uspto-grants-2009_05
特許番号
US07528160B2

反応ノート

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