3-Methyl-2-butanone → HCID 66726288, 화합물

HRID 1024493

반응식

HRID 1024493 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 66726288HCID 66726288, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-92691c7ded8f4b29ac0610f63ab42051
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08722896B2

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