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

HRID 979056

反応式

HRID 979056 の反応式
[Br:1][CH2:2][C:3](Cl)=[O:4].[CH3:6][N:7]1[CH2:16][C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[NH:9][C:8]1=[O:17].[Cl-].[Al+3].[Cl-].[Cl-]>C(=S)=S>[Br:1][CH2:2][C:3]([C:13]1[CH:14]=[C:15]2[C:10](=[CH:11][CH:12]=1)[NH:9][C:8](=[O:17])[N:7]([CH3:6])[CH2:16]2)=[O:4]

参加物

5

反応物 3

HCID 89602Bromoacetyl chlorideHCID 38465583,4-Dihydro-3-methyl-2(1H)-quinazolinoneHCID 6451240Aluminum(III) Chloride

生成物 1

HCID 138271656-(Bromoacetyl)-3,4-dihydro-3-methyl-2(1H)-quinazolinone

試薬・触媒・溶媒 1

HCID 6348Carbon Disulfide溶媒

実験手順

Bromoacetyl chloride (4.8 g) is added dropwise to a stirring solution 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 and the carbon disulfide decanted. The residue is treated with hydrochloric acid (6N) and the acidic residue poured into ice water, stirred and filtered. The filtered solid is washed with water and dried in vacuo, affording the desired product, which is used in the next step without further purification, M.P. 190°-200° C. (dec).

後処理

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

出典と根拠

ORDレコード
ord-98d69d64549a406cbdea5fa4bc3c32bb
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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