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

HRID 1247871노트

반응식

HRID 1247871 반응식
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]

참가 물질

4

반응물 2

HCID 12228Methyl IsocyanateHCID 93308Butylhydrazine hydrochloride

생성물 1

HCID 20279736N-methyl-1-butylhydrazine-carboxamide수율 82.7%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-60f69a8fd9ce4f6b98fd3ad3ff56d4f0
출처 데이터셋
uspto-grants-1985_06
특허 번호
US04521325

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