Acetic Anhydride → 1-Chloro-4-acetoxy-4-methylnonane

HRID 46963

반응식

HRID 46963 반응식
Br[CH2:2][CH2:3][CH2:4][CH2:5][CH3:6].[Mg].[Cl:8][CH2:9][CH2:10][CH2:11]C(=O)C.[C:15]([O:18][C:19](=O)[CH3:20])(=[O:17])[CH3:16]>CCOCC.O>[Cl:8][CH2:9][CH2:10][CH2:11][C:19]([O:18][C:15](=[O:17])[CH3:16])([CH3:20])[CH2:2][CH2:3][CH2:4][CH2:5][CH3:6]

참가 물질

7

반응물 4

HCID 7918Acetic AnhydrideHCID 80571-BromopentaneHCID 799932-Pentanone, 5-chloro-HCID 5462224Magnesium

생성물 1

HCID 203860911-Chloro-4-acetoxy-4-methylnonane

시약·촉매·용매 2

HCID 962Water용매HCID 3283Diethyl Ether용매

반응 조건

온도
25 °C

실험 절차

To the Grignard reagent prepared from 1-bromopentane (4.8 g., 0.04 mole) and magnesium (0.96 g., 0.04 mole) in ether is added 5-chloro-2-pentanone (6.0 g., 0.04 mole). The reaction mixture is stirred at 25° C. for 1 hour and then cooled to 15° C. Acetic anhydride (6 ml., excess) is added carefully and the solution is allowed to stand for 20 hours. Water is added, and the ether layer is separated, washed with brine, and dried over sodium sulfate. Distillation affords the title compound in 4.3 g. (46%) yield, b.p. 88° C. (0.1 mm.).

후처리

  1. temperaturecooled to 15° C
  2. waitto stand for 20 hours
  3. customthe ether layer is separated
  4. washwashed with brine
  5. dry with materialdried over sodium sulfate
  6. distillationDistillation

출처 및 근거

ORD 기록
ord-60e709a3e42e4d008d76476169273d9f
출처 데이터셋
uspto-grants-1979_11
특허 번호
US04175203

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