홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Methanol → HCID 178496795, 화합물

HRID 1067920
노트
인쇄 미리보기

반응식

HRID 1067920 반응식
CO[C:3](OC)=[N:4][NH:5][C:6]([O:8][CH3:9])=[O:7].[CH3:12][NH2:13].[CH3:14][OH:15]>>[CH3:14][O:15][CH2:12][NH:13][CH:3]=[N:4][NH:5][C:6]([O:8][CH3:9])=[O:7]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 887MethanolHCID 6329MethylamineHCID 10986557HCID 10986557, 화합물

생성물 1

HCID 178496795HCID 178496795, 화합물

실험 절차

4.77 g (25.0 mmol) of methyl N′-dimethoxymethylenehydrazinecarboxylate (85% pure) were admixed with 15.3 g of a 51% strength solution of methylamine (250 mmol) in methanol, and the mixture was stirred at room temperature for 3 days. The orange-red solution was concentrated under reduced pressure to remove excess methylamine. This gave crude methyl N′-(methoxymethylaminomethylene)hydrazinecarboxylate which was then taken up in methanol (15 ml) and, with 4.95 g (27.5 mmol) of sodium methoxide solution (30% in methanol), heated to 50° C. After 3 h 50 min, the reaction mixture was cooled to room temperature, neutralized using 2N HCl and concentrated under reduced pressure. The residue was taken up in water (6 ml) and stored overnight in a fridge. The colourless crystals were filtered off, washed with cold water and dried under reduced pressure. This gave 1.70 g (52.7%) of 5-methoxy-4-methyl-2,4-dihydro-1,2,4-triazol-3-one in the form of a colourless solid. Melting point 146-148° C.

후처리

  1. concentrationThe orange-red solution was concentrated under reduced pressure
  2. customto remove excess methylamine

출처 및 근거

ORD 기록
ord-f60190baf6944d9e859a35d28be50ca6
출처 데이터셋
uspto-grants-2001_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06248900B1

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트