Benzene → Isopropyl 11-methylthio-3,7,11-trimethyldodeca-2,4-dienoate

HRID 1605135노트

반응식

HRID 1605135 반응식
[CH3:1][S:2][C:3]([CH3:19])([CH3:18])[CH2:4][CH2:5][CH2:6][CH:7]([CH3:17])[CH2:8][CH:9]=[CH:10][C:11]([CH3:16])=[CH:12][C:13]([OH:15])=[O:14].[CH:20]1[CH:25]=CC=C[CH:21]=1.C(Cl)(=O)C(Cl)=O.C(=O)(O)[O-].[Na+]>CCOCC.C(O)(C)C>[CH3:1][S:2][C:3]([CH3:18])([CH3:19])[CH2:4][CH2:5][CH2:6][CH:7]([CH3:17])[CH2:8][CH:9]=[CH:10][C:11]([CH3:16])=[CH:12][C:13]([O:15][CH:20]([CH3:25])[CH3:21])=[O:14]

참가 물질

7

반응물 4

HCID 241BenzeneHCID 65578Oxalyl chlorideHCID 516892Sodium BicarbonateHCID 5422430711-Methylthio-3,7,11-trimethyldodeca-2,4-dienoic acid

생성물 1

HCID 54300429Isopropyl 11-methylthio-3,7,11-trimethyldodeca-2,4-dienoate

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 3776Isopropanol용매

실험 절차

To 0.6 g. of 11-methylthio-3,7,11-trimethyldodeca-2,4-dienoic acid in 10 ml. of dry benzene is added 0.23 ml. of oxalyl chloride at room temperature with stirring. After 2 hours, isopropanol (2ml.) is added and the mixture allowed to stand at room temperature for about 2 hours. Ether and saturated sodium bicarbonate is added and the organic phase separated. The organic phase is washed with aqueous sodium bicarbonate, saturated sodium chloride, dried over calcium sulfate and evaporated to yield isopropyl 11-methylthio-3,7,11-trimethyldodeca-2,4-dienoate.

후처리

  1. waitto stand at room temperature for about 2 hours
  2. customthe organic phase separated
  3. washThe organic phase is washed with aqueous sodium bicarbonate, saturated sodium chloride
  4. dry with materialdried over calcium sulfate
  5. customevaporated

출처 및 근거

ORD 기록
ord-2275bdf051b343de9dcf80ef654d801d
출처 데이터셋
uspto-grants-1976_04
특허 번호
US03948996

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