Water → 5-Bromo-2-methyl-2,3-dihydro-1-benzofuran

HRID 638361ノート

反応式

HRID 638361 の反応式
[Br:1]Br.[CH3:3][CH:4]1[O:8][C:7]2[CH:9]=[CH:10][CH:11]=[CH:12][C:6]=2[CH2:5]1.O.C(=O)(O)[O-].[Na+]>C(Cl)Cl>[Br:1][C:11]1[CH:10]=[CH:9][C:7]2[O:8][CH:4]([CH3:3])[CH2:5][C:6]=2[CH:12]=1

参加物

6

反応物 4

HCID 962WaterHCID 24408BromineHCID 1011302,3-Dihydro-2-methylbenzofuranHCID 516892Sodium Bicarbonate

生成物 1

HCID 133016015-Bromo-2-methyl-2,3-dihydro-1-benzofuran

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of 215 ml of bromine in 450 ml of methylene chloride is added dropwise over 21/2 hours to an ice-cooled mixture of 562.3 g of 2,3-dihydro-2-methylbenzo[b]furan, 1600 ml of methylene chloride, 1600 ml of water and 352.5 g of sodium bicarbonate. After the mixture has been stirred for another 11/2 hours at the same temperature, the aqueous phase is separated and extracted with two 300 ml portions of methylene chloride. The combined organic phases are washed with 2×250 ml of water, dried over sodium sulfate and concentrated. After removal of all constituents having a boiling point below 99° C. under a pressure of 8 mbar, there are obtained 750.7 g of 5-bromo-2,3-dihydro-2-methylbenzo[b]furan as residue.

後処理

  1. temperaturecooled
  2. customthe aqueous phase is separated
  3. extractionextracted with two 300 ml portions of methylene chloride
  4. washThe combined organic phases are washed with 2×250 ml of water
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated
  7. customAfter removal of all constituents

出典と根拠

ORDレコード
ord-b1b43d5a3213448383d19baeadbfb6d7
出典データセット
uspto-grants-1985_12
特許番号
US04560771

反応ノート

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