Water → 3-(4'-Butoxybenzylidene)-bornan-2-one

HRID 1995895

반응식

HRID 1995895 반응식
[C:1]12([CH3:11])[C:8]([CH3:10])([CH3:9])[CH:5]([CH2:6][CH2:7]1)[CH2:4][C:2]2=[O:3].C[O-].[Na+].[CH2:15]([O:19][C:20]1[CH:27]=[CH:26][C:23]([CH:24]=O)=[CH:22][CH:21]=1)[CH2:16][CH2:17][CH3:18].O>C1(C)C=CC=CC=1>[CH2:15]([O:19][C:20]1[CH:21]=[CH:22][C:23]([CH:24]=[C:4]2[CH:5]3[C:8]([CH3:10])([CH3:9])[C:1]([CH3:11])([CH2:7][CH2:6]3)[C:2]2=[O:3])=[CH:26][CH:27]=1)[CH2:16][CH2:17][CH3:18]

참가 물질

6

반응물 4

HCID 962WaterHCID 2537CamphorHCID 798134-ButoxybenzaldehydeHCID 10942334Sodium Methoxide

생성물 1

HCID 540235863-(4'-Butoxybenzylidene)-bornan-2-one

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A solution of 100 millimols (15.2 g) of camphor in 250 ml of toluene is heated for 1 hour at the boil with 100 mmols (5.4 g) of sodium methylate. After cooling, 100 mmols (17.8 g) of p-butoxybenzaldehyde are introduced and the mixture is heated at the reflux temperature for 4 hours. The reaction mixture is cooled and 50 ml of water are then added; the toluene phase is separated off, washed with water, dried over sodium sulphate and concentrated to dryness. The solid residue is crystallised from aqueous isopropanol. After drying, 12 g of a white owder, which melts at 62°, are collected.

후처리

  1. temperatureAfter cooling
  2. temperaturethe mixture is heated at the reflux temperature for 4 hours
  3. temperatureThe reaction mixture is cooled
  4. customthe toluene phase is separated off
  5. washwashed with water
  6. dry with materialdried over sodium sulphate
  7. concentrationconcentrated to dryness
  8. customThe solid residue is crystallised from aqueous isopropanol
  9. customAfter drying
  10. custom12 g of a white owder, which melts at 62°, are collected

출처 및 근거

ORD 기록
ord-404ba4ddbfa9498dac3c2a28f9130a1a
출처 데이터셋
uspto-grants-1983_09
특허 번호
US04406880

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