Phosphorus tribromide → HCID 19844235, 화합물

HRID 34709노트

반응식

HRID 34709 반응식
[CH2:1]([C:5]1[CH2:6][C:7]2[C:12]([C:13]=1OC)=[CH:11][C:10]1[O:16][CH2:17][O:18][C:9]=1[CH:8]=2)[CH2:2][CH2:3][CH3:4].P(Br)(Br)[Br:20]>C(Cl)(Cl)Cl>[CH2:1]([C:5]1[CH2:6][C:7]2[C:12]([C:13]=1[Br:20])=[CH:11][C:10]1[O:16][CH2:17][O:18][C:9]=1[CH:8]=2)[CH2:2][CH2:3][CH3:4]

참가 물질

4

반응물 2

HCID 24614Phosphorus tribromideHCID 198442392-n-Butyl-3-methoxy-5,6-methylenedioxyindene

생성물 1

HCID 19844235HCID 19844235, 화합물수율 68.2%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

Dissolved in 100 ml of chloroform was 9.3 g of 2-n-butyl-3-methoxy-5,6-methylenedioxyindene, followed by a dropwise addition of 15.4 g of phosphorus tribromide over 1 hour under ice cooling. After stirring the resultant mixture for further 4 hours, the reaction mixture was stirred for additional 4 hours at room temperature. The reaction mixture was washed with water, a 5% aqueous solution of sodium hydroxide and water successively, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The residue was purified by column chromatography on silica gel (eluent: a 20:1 mixture of n-hexane and ether) to give 7.6 g of 2-n-butyl-3-bromo-5,6-methylenedioxyindene having a melting point of 63.0°-64.0° C. as crystals (yield: 68%).

후처리

  1. washThe reaction mixture was washed with water
  2. dry with materiala 5% aqueous solution of sodium hydroxide and water successively, dried over anhydrous magnesium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customThe residue was purified by column chromatography on silica gel (eluent
  5. additiona 20:1 mixture of n-hexane and ether)

출처 및 근거

ORD 기록
ord-ada1fce3694045b5954ca4e93eb682d9
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04762927

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