2-Chloro-6,7-dimethoxy-4-quinazolinamine → Terazosin Hydrochloride Anhydrous

HRID 1653671

반응식

HRID 1653671 반응식
[Cl:1][C:2]1[N:11]=[C:10]([NH2:12])[C:9]2[C:4](=[CH:5][C:6]([O:15][CH3:16])=[C:7]([O:13][CH3:14])[CH:8]=2)[N:3]=1.[O:17]1[CH2:21][CH2:20][CH2:19][CH:18]1[C:22]([N:24]1[CH2:29][CH2:28][NH:27][CH2:26][CH2:25]1)=[O:23]>COC(O)C>[ClH:1].[O:17]1[CH2:21][CH2:20][CH2:19][CH:18]1[C:22]([N:24]1[CH2:25][CH2:26][N:27]([C:2]2[N:11]=[C:10]([NH2:12])[C:9]3[C:4](=[CH:5][C:6]([O:15][CH3:16])=[C:7]([O:13][CH3:14])[CH:8]=3)[N:3]=2)[CH2:28][CH2:29]1)=[O:23]

참가 물질

4

반응물 2

HCID 902352-Chloro-6,7-dimethoxy-4-quinazolinamineHCID 27346411-(Tetrahydro-2-furoyl)piperazine

생성물 1

HCID 44383Terazosin Hydrochloride Anhydrous

시약·촉매·용매 1

HCID 30156371-Methoxyethanol용매

실험 절차

To 7.00 g 2-chloro-4-amino-6,7-dimethoxyquinazoline (Lancaster Synthesis) in 50 ml methoxyethanol was added 10.8 g, tetrahydrofuroylpiperazine, and the mixture refluxed 3 hours. The clear solution was concentrated and an aqueous solution of potassium bicarbonate was added. The resultant solid that formed was filtered and washed with water. It was then added to methanol and the resulting suspension was acidified with a solution of hydrogen chloride in isopropyl alcohol. The resulting solution was concentrated and the residue crystallized from isopropyl alcohol giving 8.12 g. of product, m.p. 278°-279° C.

후처리

  1. temperaturethe mixture refluxed 3 hours
  2. concentrationThe clear solution was concentrated
  3. additionan aqueous solution of potassium bicarbonate was added
  4. customThe resultant solid that formed
  5. filtrationwas filtered
  6. washwashed with water
  7. additionIt was then added to methanol
  8. concentrationThe resulting solution was concentrated
  9. customthe residue crystallized from isopropyl alcohol giving 8.12 g

출처 및 근거

ORD 기록
ord-0e41a6faa1c04f1c9c0eadce49ddc28e
출처 데이터셋
uspto-grants-1995_04
특허 번호
US05403847

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