Bromine → 7-bromo-2,3-dihydro-1,4-benzodioxin-6-amine

HRID 723532노트

반응식

HRID 723532 반응식
[O:1]1[C:6]2[CH:7]=[CH:8][C:9]([NH2:11])=[CH:10][C:5]=2[O:4][CH2:3][CH2:2]1.[Br:12]Br>ClCCl>[Br:12][C:8]1[C:9]([NH2:11])=[CH:10][C:5]2[O:4][CH2:3][CH2:2][O:1][C:6]=2[CH:7]=1

참가 물질

4

반응물 2

HCID 24408BromineHCID 891481,4-Benzodioxan-6-ylamine

생성물 1

HCID 49832297-bromo-2,3-dihydro-1,4-benzodioxin-6-amine수율 30.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A solution of 2,3-dihydro-benzo[1,4]dioxin-6-ylamine (32 g, 212 mmol) in dichloromethane (1 liter) was treated with a solution of bromine (10.8 ml, 212 mmol) in dichloromethane (100 ml) at 0° C. After the addition the mixture was stirred at room temperature for 1 hour then washed with saturated aqueous sodium bicarbonate solution containing a small amount of sodium sulphite. The organic organic extract was dried and evaporated affording an oil that was chromatographed on silica gel eluting with dichloromethane to afford an oil (14.8 g, 30%).

후처리

  1. additionAfter the addition the mixture
  2. washthen washed with saturated aqueous sodium bicarbonate solution
  3. additioncontaining a small amount of sodium sulphite
  4. extractionThe organic organic extract
  5. customwas dried
  6. customevaporated
  7. customaffording an oil that
  8. customwas chromatographed on silica gel eluting with dichloromethane

출처 및 근거

ORD 기록
ord-ef8ab915944c458ab953ba7c763bae72
출처 데이터셋
uspto-grants-2006_11
특허 번호
US07141564B2

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