Propanoyl bromide, 2-bromo- → 6-(2-Bromopropionyl)-3,4-dihydro-3-methyl-2(1H)-quinazolinone

HRID 979057

反応式

HRID 979057 の反応式
[Br:1][CH:2]([CH3:6])[C:3](Br)=[O:4].[CH3:7][N:8]1[CH2:17][C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[NH:10][C:9]1=[O:18].[Cl-].[Al+3].[Cl-].[Cl-]>C(=S)=S>[Br:1][CH:2]([CH3:6])[C:3]([C:14]1[CH:15]=[C:16]2[C:11](=[CH:12][CH:13]=1)[NH:10][C:9](=[O:18])[N:8]([CH3:7])[CH2:17]2)=[O:4]

参加物

5

反応物 3

HCID 79047Propanoyl bromide, 2-bromo-HCID 38465583,4-Dihydro-3-methyl-2(1H)-quinazolinoneHCID 6451240Aluminum(III) Chloride

生成物 1

HCID 138271666-(2-Bromopropionyl)-3,4-dihydro-3-methyl-2(1H)-quinazolinone

試薬・触媒・溶媒 1

HCID 6348Carbon Disulfide溶媒

実験手順

2-Bromopropionyl bromide (6.7 g) is added dropwise to a stirring mixture of 3,4-dihydro-3-methyl-2(1H)-quinazolinone (2.5 g) and anhydrous aluminum chloride (4.9 g) in carbon disulfide (50 ml) under nitrogen. The reaction mixture is refluxed for five hours, cooled to RT, the carbon disulfide decanted, and the residue treated with hydrochloric acid (6N). The treated residue is poured into ice water, and the resulting suspension is stirred, filtered, the filtered solid washed with water, and dried in vacuo, affording the desired product, which is used in the next step without further purification, M.P. 150°-165° C. (dec).

後処理

  1. temperatureThe reaction mixture is refluxed for five hours
  2. customthe carbon disulfide decanted
  3. additionthe residue treated with hydrochloric acid (6N)
  4. additionThe treated residue is poured into ice water
  5. filtrationfiltered
  6. washthe filtered solid washed with water
  7. customdried in vacuo

出典と根拠

ORDレコード
ord-9da76f7a64844b85b6eca56b74afeecd
出典データセット
uspto-grants-1987_05
特許番号
US04666913

関連ノート

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