Triethylamine → 1-t-Butylazo-1-chlorocyclohexane

HRID 436728

反応式

HRID 436728 の反応式
[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]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 24526Chlorine2 回HCID 169919Cyclohexanone, 2-(1,1-dimethylethyl)hydrazone

生成物 1

HCID 233447841-t-Butylazo-1-chlorocyclohexane

試薬・触媒・溶媒 1

HCID 8003Pentane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-cec35b8d25eb457380862f8bea1cbeed
出典データセット
uspto-grants-1977_06
特許番号
US04028344

関連ノート

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