Dimethyl Sulfoxide → 1-Phenyl-1,3-octadecanedione

HRID 2225986노트

반응식

HRID 2225986 반응식
CS(C)=O.[C:5]([O:22]C)(=O)[CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH3:20].[C:24]([C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1)(=[O:26])[CH3:25]>O1CCCC1>[C:27]1([C:24](=[O:26])[CH2:25][C:5](=[O:22])[CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH3:20])[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1

참가 물질

5

반응물 3

HCID 679Dimethyl SulfoxideHCID 7410AcetophenoneHCID 8181Methyl Palmitate

생성물 1

HCID 870271-Phenyl-1,3-octadecanedione

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
0 °C

실험 절차

An apparatus as described in Example 1 is charged with 31.7 g of sodium-tert-butylate, 150 g of DMSO and 150 g of tetrahydrofuran (THF) and the mixture is cooled to 0° C. Then a mixture of 89 g of methyl palmitate and 36 g of acetophenone is added dropwise over 45 minutes. The reaction mixture is then stirred for ca. 45-60 minutes at 30° C., the solvent is removed by distillation on a rotary evaporator (bath temperature <60° C.), and the residue is taken up in 1000 ml of water. The aqueous solution is acidified with dilute hydrochloric acid and the precipitate is isolated by filtration, washed with water, and dried.

후처리

  1. additionis added dropwise over 45 minutes
  2. customthe solvent is removed by distillation on a rotary evaporator (bath temperature <60° C.)
  3. customthe precipitate is isolated by filtration
  4. washwashed with water
  5. customdried

출처 및 근거

ORD 기록
ord-68a0561f4e754eecb677d9c6c44c67e8
출처 데이터셋
uspto-grants-1994_09
특허 번호
US05344992

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