Hydrogen Bromide → 2-(1,3-Benzodioxol-5-yl)-2-bromoacetic acid

HRID 322093ノート

反応式

HRID 322093 の反応式
[BrH:1].[O:2]1[C:6]2[CH:7]=[CH:8][C:9]([CH:11](O)[C:12]([OH:14])=[O:13])=[CH:10][C:5]=2[O:4][CH2:3]1>C1(C)C=CC=CC=1.ClCCl>[O:2]1[C:6]2[CH:7]=[CH:8][C:9]([CH:11]([Br:1])[C:12]([OH:14])=[O:13])=[CH:10][C:5]=2[O:4][CH2:3]1

参加物

5

反応物 2

HCID 260Hydrogen BromideHCID 1196183',4'-Methylenedioxymandelic acid

生成物 1

HCID 113459502-(1,3-Benzodioxol-5-yl)-2-bromoacetic acid

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 6344Dichloromethane溶媒

実験手順

62% Aqueous hydrobromic acid (220 ml) was added slowly to a stirred suspension of 2-(1,3-benzodioxol-5-yl)-2-hydroxyacetic acid (see J Org Chem, 50(23), 4523-6, 1985; 82.4 g) in a mixture of toluene (500 ml) and dichloromethane (1 liter). The mixture was stirred vigorously for 4 h. The aqueous layer was separated and removed and the organics were dried (MgSO4) and concentrated to give a brown oil. The oil crystallised over a 24 h period to give 105.3 g of the title compound.

後処理

  1. customThe aqueous layer was separated
  2. customremoved
  3. dry with materialthe organics were dried (MgSO4)
  4. concentrationconcentrated
  5. customto give a brown oil
  6. customThe oil crystallised over a 24 h period

出典と根拠

ORDレコード
ord-ca7941e975254853b7dfc53b89b25352
出典データセット
uspto-grants-2001_04
特許番号
US06211223B1

反応ノート

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