Carbon Disulfide → 2-Methyl-9,10-dihydro-benzo[5,6]cyclohepta[1,2-d]oxazol-4-one

HRID 441713노트

반응식

HRID 441713 반응식
[CH3:1][C:2]1[O:3][C:4]([CH2:10][CH2:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[C:5]([C:7](Cl)=[O:8])[N:6]=1.C(=S)=S.[Cl-].[Al+3].[Cl-].[Cl-]>C(OCC)(=O)C>[CH3:1][C:2]1[O:3][C:4]2[CH2:10][CH2:11][C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=3[C:7](=[O:8])[C:5]=2[N:6]=1

참가 물질

5

반응물 3

HCID 6348Carbon DisulfideHCID 6451240Aluminum(III) ChlorideHCID 214177332-Methyl-5-(2-phenylethyl)-1,3-oxazole-4-carbonyl chloride

생성물 1

HCID 122003742-Methyl-9,10-dihydro-benzo[5,6]cyclohepta[1,2-d]oxazol-4-one

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

1.0 g. of 2-methyl-5-phenethyl-4-oxazolecarbonyl chloride (obtainable by Step D, above) in 15 ml. of carbon disulfide, 2.5 g. of anhydrous aluminum chloride added, and the mixture refluxed for 1 hour. The mixture is then cooled, poured on to ice, and extracted twice with 10 ml. portions of chloroform. The extracts are combined, dried over anhydrous sodium sulfate and evaporated (under vacuum) to obtain a solid residue, which is recyrstallized from ethyl acetate to obtain the title compound, m.p. 174°-176°.

후처리

  1. temperaturethe mixture refluxed for 1 hour
  2. temperatureThe mixture is then cooled
  3. additionpoured on to ice
  4. extractionextracted twice with 10 ml
  5. dry with materialdried over anhydrous sodium sulfate
  6. customevaporated (under vacuum)
  7. customto obtain a solid residue, which

출처 및 근거

ORD 기록
ord-180950944dca4300a9b9ddc596ec1bbd
출처 데이터셋
uspto-grants-1977_08
특허 번호
US04042596

반응 노트

불러오는 중…