Boron tribromide → HCID 19040960、化合物

HRID 2399948ノート

反応式

HRID 2399948 の反応式
C[O:2][C:3]1[CH:20]=[C:19]([O:21]C)[CH:18]=[CH:17][C:4]=1[C:5]([N:7]([CH:14]([CH3:16])[CH3:15])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)=[O:6].B(Br)(Br)Br>ClCCl>[OH:2][C:3]1[CH:20]=[C:19]([OH:21])[CH:18]=[CH:17][C:4]=1[C:5]([N:7]([CH:14]([CH3:16])[CH3:15])[C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1)=[O:6]

参加物

4

反応物 2

HCID 25134Boron tribromideHCID 19040985HCID 19040985、化合物

生成物 1

HCID 19040960HCID 19040960、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A stirred solution of 2,4-dimethoxy-N-(1-methylethyl)-N-phenylbenzamide (2.4 g, 8.03 mmol) in 10 ml of dichloromethane at 0° C. was treated with 1N boron tribromide (33.2 mL, 33.2 mmol) and stirred at room temperature for 1 hour. The reaction is poured in to the ice water. After stirring for 15 minutes, the reaction was partitioned between ethyl acetate and brine, dried over magnesium sulfate and concentrated in vacuo to afford yellow foam. This material is purified by chromatography on silica gel (70 g) with 3-5% methanol/dichloromethane as the eluent to afford 2,4-dihydroxy-N-(1-methylethyl)-N-phenylbenzamide as colorless foam.

後処理

  1. stirringAfter stirring for 15 minutes
  2. customthe reaction was partitioned between ethyl acetate and brine
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated in vacuo
  5. customto afford yellow foam
  6. customThis material is purified by chromatography on silica gel (70 g) with 3-5% methanol/dichloromethane as the eluent

出典と根拠

ORDレコード
ord-07b264b656a64eaf925a6e38843ca29b
出典データセット
uspto-grants-1995_09
特許番号
US05451700

反応ノート

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