Methyl chloroformate → Methyl (2-tert-butyl-4-bromophenyl) carbonate

HRID 73997

反応式

HRID 73997 の反応式
[C:1]([C:5]1[CH:10]=[C:9]([Br:11])[CH:8]=[CH:7][C:6]=1[OH:12])([CH3:4])([CH3:3])[CH3:2].CCN(CC)CC.Cl[C:21]([O:23][CH3:24])=[O:22]>ClCCl>[C:21](=[O:22])([O:12][C:6]1[CH:7]=[CH:8][C:9]([Br:11])=[CH:10][C:5]=1[C:1]([CH3:4])([CH3:2])[CH3:3])[O:23][CH3:24]

参加物

5

反応物 3

HCID 6586Methyl chloroformateHCID 8471TriethylamineHCID 970684-Bromo-2-tert-butylphenol

生成物 1

HCID 57470234Methyl (2-tert-butyl-4-bromophenyl) carbonate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

To a solution of 2-t-butyl-4-bromophenol (380 g, 1.67 mol) in dichloromethane (1000 mL) was added Et3N (202 g, 2 mol) at room temperature. Methyl chloroformate (155 mL) was added dropwise to the above solution at 0° C. After addition, the mixture was stirred at 0° C. for 2 h., quenched with saturated ammonium chloride solution and diluted with water. The organic layer was separated and washed with water and brine, dried over Na2SO4, and concentrated to provide the crude methyl (2-tert-butyl-4-bromophenyl) carbonate (470 g), which was used without further purification.

後処理

  1. additionAfter addition
  2. customquenched with saturated ammonium chloride solution
  3. additiondiluted with water
  4. customThe organic layer was separated
  5. washwashed with water and brine
  6. dry with materialdried over Na2SO4
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-22d937dff14640f0857c10acfa257ab0
出典データセット
uspto-grants-2014_09
特許番号
US08829204B2

関連ノート

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