Triethylamine → 1-t-Butylazo-1-chlorocyclohexane

HRID 436728

반응식

HRID 436728 반응식
[C:1]([NH:5][N:6]=[C:7]1[CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]1)([CH3:4])([CH3:3])[CH3:2].C(N(CC)CC)C.[Cl:20]Cl>CCCCC>[C:1]([N:5]=[N:6][C:7]1([Cl:20])[CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]1)([CH3:4])([CH3:2])[CH3:3]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 24526Chlorine2회HCID 169919Cyclohexanone, 2-(1,1-dimethylethyl)hydrazone

생성물 1

HCID 233447841-t-Butylazo-1-chlorocyclohexane

시약·촉매·용매 1

HCID 8003Pentane용매

실험 절차

To a stirred solution of 252 grams (1.5 moles) of cyclohexanone t-butylhydrazone and 160 grams (1.5 moles) of triethylamine in 1200 ml pentane in a 3 liter 4 neck flask equipped with a mechanical stirrer, thermometer and gas inlet tube, was added 107 grams (1.5 moles) of chlorine gas, holding the temperature at -10° to 0° C. After the chlorine addition was complete, the reaction mixture was stirred an additional 15 minutes and the insoluble triethylamine hydrochloride filtered off. The filter cake was washed with an additional 300 ml pentane and the filtrate stripped of pentane under reduced pressure. The yield of 1-t-butylazo-1-chlorocyclohexane was 266 grams (87.5% crude yield).

후처리

  1. customat -10° to 0° C
  2. filtrationthe insoluble triethylamine hydrochloride filtered off
  3. washThe filter cake was washed with an additional 300 ml pentane

출처 및 근거

ORD 기록
ord-cec35b8d25eb457380862f8bea1cbeed
출처 데이터셋
uspto-grants-1977_06
특허 번호
US04028344

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