Methylhydrazine → 4-[1-(t-Butylazo)cyclohexyl]-2-methylsemicarbazide

HRID 436749ノート

反応式

HRID 436749 の反応式
[C:1]([N:5]=[N:6][C:7]1([N:13]=[C:14]=[O:15])[CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]1)([CH3:4])([CH3:3])[CH3:2].[CH3:16][NH:17][NH2:18].[N-]=C=O>CCCCC>[C:1]([N:5]=[N:6][C:7]1([NH:13][C:14](=[O:15])[N:17]([CH3:16])[NH2:18])[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 6061MethylhydrazineHCID 105034IsocyanateHCID 214311721-t-Butylazo-1-isocyanatocyclohexane

生成物 1

HCID 214311464-[1-(t-Butylazo)cyclohexyl]-2-methylsemicarbazide

試薬・触媒・溶媒 1

HCID 8003Pentane溶媒

反応条件

温度
5 °C

実験手順

To 8.2 grams (0.0392 moles) of 1-t-butylazo-1-isocyanatocyclohexane stirred with a magnetic stirrer in a 50 ml erlenmeyer flask and cooled to 5° C. was added 1.82 grams (0.0392 moles) of methylhydrazine. The reaction was very rapid and exothermic and became quite viscous. The reaction mixture was diluted with pentane and stirred for an additional 60 minutes at room temperature. The pentane was evaporated under reduced pressure leaving 9.0 grams (90% crude yield) of a yellow solid. The product melted at 169°-171° C. with decomposition. The infrared spectrum of the product contained a strong carbonyl band at 1660 cm-1 and a moderate NH band at 3320 cm-1. The isocyanate band at 2225 cm-1 was absent.

後処理

  1. customThe pentane was evaporated under reduced pressure
  2. customleaving 9.0 grams (90% crude yield) of a yellow solid

出典と根拠

ORDレコード
ord-8d416c253721430bb3e24f8c083b70fb
出典データセット
uspto-grants-1977_06
特許番号
US04028344

反応ノート

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