5-Methyl-2-hexanone → 3-Chloro-5-methylhexan-2-one

HRID 1954651노트

반응식

HRID 1954651 반응식
[CH3:1][CH:2]([CH3:8])[CH2:3][CH2:4][C:5](=[O:7])[CH3:6].S(Cl)([Cl:12])(=O)=O>CCCCCC>[Cl:12][CH:4]([CH2:3][CH:2]([CH3:8])[CH3:1])[C:5](=[O:7])[CH3:6]

참가 물질

4

반응물 2

HCID 80345-Methyl-2-hexanoneHCID 24648Sulfuryl chloride2회

생성물 1

HCID 109756493-Chloro-5-methylhexan-2-one수율 90.4%

시약·촉매·용매 1

HCID 8058Hexane용매

실험 절차

To a refluxing solution of 750 g (6.58 mol) 5-methyl-2-hexanone in 1.13 1 n-hexane at 65° C., 1.06 kg (7.89 mol) sulfuryl chloride was added over a period of 2 h. After complete addition of the sulfuryl chloride, the reaction mixture was allowed to cool to room temperature, was washed 4 times with 150 ml H2O, dried (MgSO4) and concentrated in vacuo. The residue was distilled over a 5 cm Vigreux-column (80 mbar, 67-76° C.) to give 884 g of 3-chloro-5-methyl-2-hexanone in the form of a yellowish liquid (purity: 88%, impurity: 11% 3,3-dichloro-5-methyl-2-hexanone).

후처리

  1. washwas washed 4 times with 150 ml H2O
  2. dry with materialdried (MgSO4)
  3. concentrationconcentrated in vacuo
  4. distillationThe residue was distilled over a 5 cm Vigreux-column (80 mbar, 67-76° C.)

출처 및 근거

ORD 기록
ord-b3fac65a71a8453b92b671026ec1c781
출처 데이터셋
uspto-grants-2000_09
특허 번호
US06123974

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