Boron tribromide → HCID 22292779、化合物

HRID 967254ノート

反応式

HRID 967254 の反応式
[F:1][C:2]([F:21])([F:20])[C:3]([N:5]1[CH2:11][CH:10]([CH3:12])[C:9]2[CH:13]=[C:14]([Cl:19])[C:15]([O:17]C)=[CH:16][C:8]=2[CH2:7][CH2:6]1)=[O:4].B(Br)(Br)Br>ClCCl>[F:20][C:2]([F:1])([F:21])[C:3]([N:5]1[CH2:11][CH:10]([CH3:12])[C:9]2[CH:13]=[C:14]([Cl:19])[C:15]([OH:17])=[CH:16][C:8]=2[CH2:7][CH2:6]1)=[O:4]

参加物

4

反応物 2

HCID 25134Boron tribromideHCID 22292769HCID 22292769、化合物

生成物 1

HCID 22292779HCID 22292779、化合物収率 52%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of N-trifluoroacetyl-8-chloro-7-methoxy-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine (48 mg, 0.15 mmol) in dichloromethane (2 mL) was treated with BBr3 (0.30 mL of a 1.0M solution in CH2Cl2, 0.30 mmol) and stirred overnight at 20 C. The excess BBr3 was quenched with water and the resulting mixture diluted with ether (20 mL), washed with Na2CO3 (10 mL) and brine (10 mL), dried with Na2SO4 and concentrated. Flash chromatography (15% EtOAc in hexane, silica) resulted in 24 mg of a white solid. MS calculated for C13H13ClF3NO2+H: 308, observed: 308.

後処理

  1. customThe excess BBr3 was quenched with water
  2. additionthe resulting mixture diluted with ether (20 mL)
  3. washwashed with Na2CO3 (10 mL) and brine (10 mL)
  4. dry with materialdried with Na2SO4
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-cfb18275c9fe4b9ebb4bab9c95442b2e
出典データセット
uspto-grants-2005_10
特許番号
US06953787B2

反応ノート

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