Triethylamine → Ethyl 3-ethoxy-3-imino-2-(cyclopropyloxyimino)propionate

HRID 1074340

반응식

HRID 1074340 반응식
[C:1]([C:4](=[N:10][O:11][CH:12]1[CH2:14][CH2:13]1)[C:5]([O:7][CH2:8][CH3:9])=[O:6])(=[O:3])[NH2:2].F[B-](F)(F)F.[CH2:20]([O+](CC)CC)[CH3:21].C(N(CC)CC)C>C(Cl)Cl.C(OC(C)C)(C)C>[CH2:20]([O:3][C:1](=[NH:2])[C:4](=[N:10][O:11][CH:12]1[CH2:13][CH2:14]1)[C:5]([O:7][CH2:8][CH3:9])=[O:6])[CH3:21]

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 2723982Triethyloxonium tetrafluoroborateHCID 54332569Ethyl 2-carbamoyl-2-(cyclopropyloxyimino)acetate

생성물 1

HCID 54045971Ethyl 3-ethoxy-3-imino-2-(cyclopropyloxyimino)propionate수율 69.5%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 7914Diisopropyl Ether용매

실험 절차

A mixture of ethyl 2-carbamoyl-2-(cyclopropyloxyimino)acetate (syn isomer)(84.1 g) and triethyloxonium fluoroborate (11.5 g) in methylene chloride (110 ml) was stirred at ambient temperature for 16 hours. To the mixture was added triethylamine (17 ml) under ice-cooling. The mixture was washed with water, dried over sodium sulfate, and concentrated in vacuo to give a residue. The residue was dissolved in diisopropyl ether. The solution was washed with water, dried over sodium sulfate, and concentrated in vacuo to give ethyl 3-ethoxy-3-imino-2-(cyclopropyloxyimino)propionate (syn isomer) (9.60 g) as an oil.

후처리

  1. temperaturecooling
  2. washThe mixture was washed with water
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated in vacuo
  5. customto give a residue
  6. washThe solution was washed with water
  7. dry with materialdried over sodium sulfate
  8. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-9b55814a15714c82b1b99405d98beb96
출처 데이터셋
uspto-grants-1990_11
특허 번호
US04973699

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