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O-Toluidine → 4-(N-methylphenylamino)-2-(2-methylphenylamino)-6-methoxyquinazoline hydrochloride

HRID 973578
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반응식

HRID 973578 반응식
[Cl:1][C:2]1[N:11]=[C:10]([N:12]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[CH3:13])[C:9]2[C:4](=[CH:5][CH:6]=[C:7]([O:20][CH3:21])[CH:8]=2)[N:3]=1.[NH2:22][C:23]1[C:24]([CH3:29])=[CH:25][CH:26]=[CH:27][CH:28]=1.C(O)C.Cl>C(O)C>[ClH:1].[CH3:13][N:12]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[C:10]1[C:9]2[C:4](=[CH:5][CH:6]=[C:7]([O:20][CH3:21])[CH:8]=2)[N:3]=[C:2]([NH:22][C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=2[CH3:29])[N:11]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7242O-ToluidineHCID 100861382-Chloro-4-(N-methylphenylamino)-6-methoxyquinazolineHCID 21887872Ethanol hydrochloride

생성물 1

HCID 679259664-(N-methylphenylamino)-2-(2-methylphenylamino)-6-methoxyquinazoline hydrochloride수율 57.7%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 2-chloro-4-(N-methylphenylamino)-6methoxyquinazoline (5.4 g, 0.027M), o-toluidine (4.28 g, 0.04M) in ethanol (50 ml) was heated in a Berchof pressure vessel at 140° for 5 hours (maximum pressure 40 psi). After cooling, ethanol/HCl was added and the solid which crystallised out was filtered off and recrystallised from isopropanol/ether to yield the title compound (4.23 g, m.p. 258°-260°).

후처리

  1. temperaturewas heated in a Berchof pressure vessel at 140° for 5 hours (maximum pressure 40 psi)
  2. temperatureAfter cooling
  3. customthe solid which crystallised out
  4. filtrationwas filtered off
  5. customrecrystallised from isopropanol/ether

출처 및 근거

ORD 기록
ord-f4874eb13583451e8289090777161ac8
출처 데이터셋
uspto-grants-1991_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05064833

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