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

HRID 970389노트

반응식

HRID 970389 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 litre) 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 extract was dried and evaporated to 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 extract
  5. customwas dried
  6. customevaporated to an oil that
  7. customwas chromatographed on silica gel eluting with dichloromethane

출처 및 근거

ORD 기록
ord-b0528b41507247069c02e94313101cc8
출처 데이터셋
uspto-grants-2007_12
특허 번호
US07312212B2

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