Boron tribromide → HCID 178497536、化合物

HRID 2085753ノート

反応式

HRID 2085753 の反応式
C[O:2][C:3]1[N:8]=[CH:7][C:6]([C:9]2[CH:18]=[CH:17][C:12]([C:13]([O:15][CH3:16])=[O:14])=[CH:11][CH:10]=2)=[CH:5][CH:4]=1.B(Br)(Br)Br>ClCCl>[OH:2][C:3]1[N:8]=[CH:7][C:6]([C:9]2[CH:18]=[CH:17][C:12]([C:13]([O:15][CH3:16])=[O:14])=[CH:11][CH:10]=2)=[CH:5][CH:4]=1

参加物

4

反応物 2

HCID 25134Boron tribromideHCID 4674260Methyl 4-(6-methoxy-3-pyridinyl)benzoate

生成物 1

HCID 178497536HCID 178497536、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of Example 252D (0.5 g, 2.2 mmol) in dichloromethane at −78° C. was treated with 1M BBr3 in dichloromethane (15 mL), warm to room temperature, and stirred for 18 hours. The reaction was quenched with methanol (5 mL), diluted with dichloromethane (100 mL), washed with water (30 mL), brine (30 mL), dried (Na2SO4), filtered, and concentrated. The concentrate was purified by flash column chromatography on silica gel with 2:1 hexanes/ethyl acetate to provide the desired product. MS (ESI) m/e 228, 230 (M−H)−, (M+H)+.

後処理

  1. customThe reaction was quenched with methanol (5 mL)
  2. additiondiluted with dichloromethane (100 mL)
  3. washwashed with water (30 mL), brine (30 mL)
  4. dry with materialdried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe concentrate was purified by flash column chromatography on silica gel with 2:1 hexanes/ethyl acetate

出典と根拠

ORDレコード
ord-567b9eaeb62c48ceaac794b68f157b34
出典データセット
uspto-grants-2004_04
特許番号
US06720338B2

反応ノート

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