Bromoacetyl chloride → 6-(2-Bromoacetyl)-3,4-dihydro-4-methyl-2(1H)-quinazolinone

HRID 979058ノート

反応式

HRID 979058 の反応式
[Br:1][CH2:2][C:3](Cl)=[O:4].[CH3:6][CH:7]1[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[NH:10][C:9](=[O:17])[NH:8]1.[Cl-].[Al+3].[Cl-].[Cl-]>C(=S)=S>[Br:1][CH2:2][C:3]([C:14]1[CH:15]=[C:16]2[C:11](=[CH:12][CH:13]=1)[NH:10][C:9](=[O:17])[NH:8][CH:7]2[CH3:6])=[O:4]

参加物

5

反応物 3

HCID 89602Bromoacetyl chlorideHCID 6451240Aluminum(III) ChlorideHCID 123607574-Methyl-3,4-dihydro-1H-quinazolin-2-one

生成物 1

HCID 138271676-(2-Bromoacetyl)-3,4-dihydro-4-methyl-2(1H)-quinazolinone

試薬・触媒・溶媒 1

HCID 6348Carbon Disulfide溶媒

実験手順

2-Bromoacetyl chloride (9.7 g) is added dropwise to a stirred mixture of 3,4-dihydro-4-methyl-2(1H)-quinazolinone (5 g), anhydrous aluminum chloride (10.3 g) and carbon disulfide (100 ml) under nitrogen. The reaction mixture is refluxed for about 18 hours, the carbon disulfide decanted, and the residue treated with hydrochloric acid (6N) and ethyl acetate. The layers are separated, and the aqueous layer extracted with ethyl acetate and the combined ethyl acetate extracts washed with sat'd. aqueous sodium bicarbonate and water and dried. The dried organic extract is filtered and the filtrate evaporated, affording the desired product as a solid, which is used without further purification, M.P. 188°-190° C.

後処理

  1. temperatureThe reaction mixture is refluxed for about 18 hours
  2. customthe carbon disulfide decanted
  3. additionthe residue treated with hydrochloric acid (6N) and ethyl acetate
  4. customThe layers are separated
  5. extractionthe aqueous layer extracted with ethyl acetate
  6. washthe combined ethyl acetate extracts washed with sat'd
  7. dry with materialaqueous sodium bicarbonate and water and dried
  8. extractionThe dried organic extract
  9. filtrationis filtered
  10. customthe filtrate evaporated

出典と根拠

ORDレコード
ord-23fbc969c7b541e596df8367f33737b4
出典データセット
uspto-grants-1987_05
特許番号
US04666913

反応ノート

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