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

HRID 73997

반응식

HRID 73997 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-22d937dff14640f0857c10acfa257ab0
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08829204B2

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