Methylamine → 2-Methyl-2,7-diazaspiro[4.4]nonane-1,3,8-trione

HRID 620862노트

반응식

HRID 620862 반응식
C([O:3][C:4]([C:6]1([CH2:12][C:13]([O:15]CC)=O)[CH2:10][C:9](=[O:11])[NH:8][CH2:7]1)=O)C.[CH3:18][NH2:19]>>[CH3:18][N:19]1[C:13](=[O:15])[CH2:12][C:6]2([CH2:10][C:9](=[O:11])[NH:8][CH2:7]2)[C:4]1=[O:3]

참가 물질

3

반응물 2

HCID 6329MethylamineHCID 12691859Ethyl 3-(2-ethoxy-2-oxoethyl)-5-oxopyrrolidine-3-carboxylate

생성물 1

HCID 42826302-Methyl-2,7-diazaspiro[4.4]nonane-1,3,8-trione

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온도
220 °C

실험 절차

A solution of 20.3 g (0.084 mole) 3-ethoxycarbonyl-5-oxo-3-pyrrolidineacetic acid, ethyl ester [J. Org. Chem., 46, 2757 (1981)]in 40 ml of 40% aqueous methylamine was stirred at room temperature overnight, then placed in an oil bath and gradually heated to 220° C. over 30 minutes allowing volatiles to distill from the open flask. The crude product was crystallized from ethanol to afford 12.6 g of 2-methyl-2,7-diazaspiro[4.4]nonane-1,3,8-trione, mp 201°-204° C.

후처리

  1. customplaced in an oil bath
  2. distillationto distill from the open flask
  3. customThe crude product was crystallized from ethanol

출처 및 근거

ORD 기록
ord-9b2a0eea7e8c4c1abb0114df39ca93b0
출처 데이터셋
uspto-grants-1989_04
특허 번호
US04822801

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