Ethyl chloroformate → 2-Ethenyl-4,4-dimethyl-1,3-oxazol-5(4H)-one

HRID 452282노트

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HRID 452282 반응식
[C:1]([CH2:5][NH:6][C@H:7]([C:9]([OH:11])=[O:10])[CH3:8])(=O)[CH:2]=C.Cl[C:13](OCC)=O>>[CH3:13][C:7]1([CH3:8])[N:6]=[C:5]([CH:1]=[CH2:2])[O:10][C:9]1=[O:11]

참가 물질

3

반응물 2

HCID 10928Ethyl chloroformateHCID 57278894HCID 57278894, 화합물

생성물 1

HCID 98127942-Ethenyl-4,4-dimethyl-1,3-oxazol-5(4H)-one

반응 조건

온도
-78 °C

실험 절차

2-Vinyl-4,4-Dimethylazlactone (VDM) was prepared from N-acryloylmethylalanine (S. M. Heilmann and H. K. Smith II, J. Appl. Polym. Sci., 24, 1551 (1979)) by the Taylor and Platt procedure (L. D. Taylor and T. E. Platt, J. Polym. Sci. Polym. Lett. Ed., 7, 597 (1969)) with ethyl chloroformate as the dehydrating agent. A modified workup procedure was used in which, instead of cooling the filtrate to crystallize the product, the filtrate was concentrated on a rotary evaporator, and the crude product was distilled just above room temperature at 0.5 Torr. Receiving flasks were cooled to −78° C. to collect the product. Typical distilled yields were approximately 80%.

후처리

  1. temperatureinstead of cooling the filtrate
  2. customto crystallize the product
  3. concentrationthe filtrate was concentrated on a rotary evaporator
  4. distillationthe crude product was distilled just above room temperature at 0.5 Torr
  5. customto collect the product
  6. distillationTypical distilled
  7. customyields

출처 및 근거

ORD 기록
ord-60b61a9f78fc43a9ac1283bfb1c25cc0
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08491749B2

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