Methyl Isocyanate → N-methyl-1-butylhydrazine-carboxamide

HRID 1247871ノート

反応式

HRID 1247871 の反応式
Cl.[CH2:2]([NH:6][NH2:7])[CH2:3][CH2:4][CH3:5].[CH3:8][N:9]=[C:10]=[O:11]>O1CCCC1>[CH3:8][NH:9][C:10]([N:6]([CH2:2][CH2:3][CH2:4][CH3:5])[NH2:7])=[O:11]

参加物

4

反応物 2

HCID 12228Methyl IsocyanateHCID 93308Butylhydrazine hydrochloride

生成物 1

HCID 20279736N-methyl-1-butylhydrazine-carboxamide収率 82.7%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A suspension of 2.42 g n-butylhydrazine hydrochloride in 15 mL tetrahydrofuran was degassed and stirred under nitrogen with cooling (water bath) while 1.68 g of powdered potassium hydroxide was added. Stirring and cooling continued as 0.86 g (0.015 mole) methyl isocyanate in 15 mL tetrahydrofuran was added dropwise. The resulting mixture was allowed to stir at room temperature overnight. The solution was filtered and the filtrate evaporated to yield a colorless liquid. Vacuum distillation gave 82.7% N-methyl-1-butylhydrazine-carboxamide, b.p. 116°-118° C. at 0.06 torr. The compound crystallized upon standing m.p. 48°-50° C. Its structure was confirmed by NMR analysis.

後処理

  1. customwas degassed
  2. temperaturewith cooling (water bath) while 1.68 g of powdered potassium hydroxide
  3. additionwas added
  4. stirringStirring
  5. temperaturecooling
  6. additionwas added dropwise
  7. stirringto stir at room temperature overnight
  8. filtrationThe solution was filtered
  9. customthe filtrate evaporated
  10. customto yield a colorless liquid
  11. distillationVacuum distillation

出典と根拠

ORDレコード
ord-60f69a8fd9ce4f6b98fd3ad3ff56d4f0
出典データセット
uspto-grants-1985_06
特許番号
US04521325

反応ノート

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