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

HRID 441713ノート

反応式

HRID 441713 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-180950944dca4300a9b9ddc596ec1bbd
出典データセット
uspto-grants-1977_08
特許番号
US04042596

反応ノート

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