Potassium Carbonate → 2,4-Diamino-5-chloro-6-[5-chloro-2-(pyridin-2-ylmethoxy)phenyl]quinazoline

HRID 52625

반응식

HRID 52625 반응식
[NH2:1][C:2]1[N:11]=[C:10]([NH2:12])[C:9]2[C:4](=[CH:5][CH:6]=[C:7]([C:14]3[CH:19]=[C:18]([Cl:20])[CH:17]=[CH:16][C:15]=3[OH:21])[C:8]=2[Cl:13])[N:3]=1.Cl.[N:23]1[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=1[CH2:29]Cl.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[NH2:1][C:2]1[N:11]=[C:10]([NH2:12])[C:9]2[C:4](=[CH:5][CH:6]=[C:7]([C:14]3[CH:19]=[C:18]([Cl:20])[CH:17]=[CH:16][C:15]=3[O:21][CH2:29][C:24]3[CH:25]=[CH:26][CH:27]=[CH:28][N:23]=3)[C:8]=2[Cl:13])[N:3]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 23392Picolyl chloride hydrochlorideHCID 543690952,4-Diamino-5-chloro-6-(5-chloro-2-hydroxyphenyl)quinazoline

생성물 1

HCID 541271462,4-Diamino-5-chloro-6-[5-chloro-2-(pyridin-2-ylmethoxy)phenyl]quinazoline수율 72.8%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Under a nitrogen atmosphere, a stirred solution of 0.5 gram (0.002 mole) of 2,4-diamino-5-chloro-6-(5-chloro-2-hydroxyphenyl)quinazoline, 0.3 gram (0.002 mole) of pyridin-2-ylmethyl chloride hydrochloride, and 0.5 gram (0.004 mole) of potassium carbonate in 5 mL of N,N-dimethylformamide was heated at 60° C. for about 24 hours. After this time, the reaction mixture was concentrated under reduced pressure to a residue. The residue was taken up in 100 mL of water and was stirred for about 2 hours. The resultant solid was collected by filtration, yielding 0.6 gram of 2,4-diamino-5-chloro-6-[5-chloro-2-(pyridin-2-ylmethoxy)phenyl]quinazoline. The NMR spectrum was consistent with the proposed structure.

후처리

  1. concentrationAfter this time, the reaction mixture was concentrated under reduced pressure to a residue
  2. filtrationThe resultant solid was collected by filtration

출처 및 근거

ORD 기록
ord-4e7589615bc34f8e9e23220e577c58c5
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05616718

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