Dimethylformamide dimethyl acetal → Methyl alpha-[(dimethylamino)methylene]-1H-1,2,3-triazole-1-acetate

HRID 241604노트

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HRID 241604 반응식
CO[CH:3](OC)[N:4]([CH3:6])[CH3:5].[N:9]1([C:14](=C)[C:15]([O:17][CH3:18])=[O:16])[CH:13]=[CH:12][N:11]=[N:10]1>>[CH3:6][N:4]([CH3:5])[CH:3]=[C:14]([N:9]1[CH:13]=[CH:12][N:11]=[N:10]1)[C:15]([O:17][CH3:18])=[O:16]

참가 물질

3

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HCID 78373Dimethylformamide dimethyl acetalHCID 69669790HCID 69669790, 화합물

생성물 1

HCID 69669700Methyl alpha-[(dimethylamino)methylene]-1H-1,2,3-triazole-1-acetate

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온도
55 °C

실험 절차

522 g of dimethylformamide dimethyl acetal were added to 400 g of methyl 2-(1H-1,2,3-triazol-1-yl)acrylate, and the mixture was heated to the boil. Low-boiling components formed were distilled off. After 4 h, the mixture was cooled to 55° C., and 1050 ml of methyl tert-butyl ether/2-propanol (3:1 v/v) were metered in. The resulting suspension was cooled to 22° C. and filtered. The filter cake was repeatedly washed with methyl tert-butyl ether and dried under reduced pressure at 40° C. This gave 493 g of the title compound as a solid.

후처리

  1. temperaturethe mixture was heated to the boil
  2. customLow-boiling components formed
  3. distillationwere distilled off
  4. temperatureThe resulting suspension was cooled to 22° C.
  5. filtrationfiltered
  6. washThe filter cake was repeatedly washed with methyl tert-butyl ether
  7. customdried under reduced pressure at 40° C

출처 및 근거

ORD 기록
ord-075b37b3fcd445aabe31a1f217242541
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08653074B2

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