3-Methyl-2-butanone → HCID 66726288、化合物

HRID 1024493

反応式

HRID 1024493 の反応式
[O:1]1[C:7]2[CH:8]=[CH:9][C:10]([CH:12]=O)=[CH:11][C:6]=2[O:5][CH2:4][CH2:3][CH2:2]1.[CH3:14][CH:15]([CH3:19])[C:16](=[O:18])[CH3:17].[OH-].[Na+]>CO>[O:1]1[C:7]2[CH:8]=[CH:9][C:10]([CH:12]=[CH:17][C:16](=[O:18])[CH:15]([CH3:19])[CH3:14])=[CH:11][C:6]=2[O:5][CH2:4][CH2:3][CH2:2]1

参加物

5

反応物 3

HCID 112513-Methyl-2-butanoneHCID 14798Sodium HydroxideHCID 27763883,4-dihydro-2H-1,5-benzodioxepine-7-carbaldehyde

生成物 1

HCID 66726288HCID 66726288、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

The MeOH (5 mL) solution of 3,4-dihydro-2H-1,5-benzodioxepine-7-carbaldehyde (445 mg) and 3-methyl-2-butanone (195 mg) was treated with aq. sodium hydroxide (1N, 1 ml) and the mixture was stirred for 24 hours. The reaction was partitioned between 10 ml water and 40 ml ethyl acetate. The organic layer was then sequentially washed with aq. hydrochloric acid (1N, 20 ml), water (20 ml), and Brine (20 ml) and then concentrated under reduced pressure. The residue was purified with flash chromatography on silica (33% ethyl acetate in hexane) to give the desired product as a white crystal.

後処理

  1. customThe reaction was partitioned between 10 ml water and 40 ml ethyl acetate
  2. washThe organic layer was then sequentially washed with aq. hydrochloric acid (1N, 20 ml), water (20 ml), and Brine (20 ml)
  3. concentrationconcentrated under reduced pressure
  4. customThe residue was purified with flash chromatography on silica (33% ethyl acetate in hexane)

出典と根拠

ORDレコード
ord-92691c7ded8f4b29ac0610f63ab42051
出典データセット
uspto-grants-2014_05
特許番号
US08722896B2

関連ノート

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