Methyl 2-nitroacetate → Methyl nitro(1,3-oxazinan-2-ylidene)acetate

HRID 1283936

반응식

HRID 1283936 반응식
CS[C:3]1[O:4][CH2:5][CH2:6][CH2:7][N:8]=1.[N+:9]([CH2:12][C:13]([O:15][CH3:16])=[O:14])([O-:11])=[O:10]>[Cl-].[Zn+2].[Cl-]>[N+:9]([C:12](=[C:3]1[NH:8][CH2:7][CH2:6][CH2:5][O:4]1)[C:13]([O:15][CH3:16])=[O:14])([O-:11])=[O:10]

참가 물질

4

반응물 2

HCID 17206Methyl 2-nitroacetateHCID 218167185,6-dihydro-2-(methylthio)-4H-1,3-oxazine

생성물 1

HCID 71444191Methyl nitro(1,3-oxazinan-2-ylidene)acetate

시약·촉매·용매 1

HCID 3007855Zincchloride촉매

실험 절차

A mixture of 25 g of 5,6-dihydro-2-(methylthio)-4H-1,3-oxazine (Clapp, et al., J. Heterocyclic Chemistry, 5, 107 (1968)), 25 g of methyl nitroacetate and a catalytic amount of zinc chloride was heated to 90° over one hour and maintained at that temperature for an additional hour. The mixture then was cooled and triturated with ether to effect crystallization. The solid was recrystallized from ethanol to give methyl nitro(tetrahydro-2H-1,3-oxazin-2-ylidene)acetate (1A), as a yellow solid, m.p.: 132°-3°.

후처리

  1. temperaturemaintained at that temperature for an additional hour
  2. temperatureThe mixture then was cooled
  3. customtriturated with ether
  4. customcrystallization
  5. customThe solid was recrystallized from ethanol

출처 및 근거

ORD 기록
ord-c9185385c0a245acabbfac2212c48638
출처 데이터셋
uspto-grants-1976_08
특허 번호
US03976772

연결된 노트

불러오는 중…