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

HRID 970389ノート

反応式

HRID 970389 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-b0528b41507247069c02e94313101cc8
出典データセット
uspto-grants-2007_12
特許番号
US07312212B2

反応ノート

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