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

HRID 979056

반응식

HRID 979056 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6348Carbon Disulfide용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-98d69d64549a406cbdea5fa4bc3c32bb
출처 데이터셋
uspto-grants-1987_05
특허 번호
US04666913

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