Phosphorus tribromide → HCID 19844235、化合物

HRID 34709ノート

反応式

HRID 34709 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

HCID 19844235HCID 19844235、化合物収率 68.2%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-ada1fce3694045b5954ca4e93eb682d9
出典データセット
uspto-grants-1988_08
特許番号
US04762927

反応ノート

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