Triethylamine → 2-Chloro-N-[(2,2-dimethyl-1,3-dioxolan-4-yl)methyl]-6-methylquinazolin-4-amine

HRID 540252노트

반응식

HRID 540252 반응식
[Cl:1][C:2]1[N:11]=[C:10](Cl)[C:9]2[C:4](=[CH:5][CH:6]=[C:7]([CH3:13])[CH:8]=2)[N:3]=1.C(N(CC)CC)C.[CH3:21][C:22]1([CH3:29])[O:26][CH:25]([CH2:27][NH2:28])[CH2:24][O:23]1>CO.C(OCC)(=O)C>[Cl:1][C:2]1[N:11]=[C:10]([NH:28][CH2:27][CH:25]2[CH2:24][O:23][C:22]([CH3:29])([CH3:21])[O:26]2)[C:9]2[C:4](=[CH:5][CH:6]=[C:7]([CH3:13])[CH:8]=2)[N:3]=1

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 41223491,3-Dioxolane-4-methanamine, 2,2-dimethyl-HCID 142564832,4-Dichloro-6-methylquinazoline

생성물 1

HCID 866914222-Chloro-N-[(2,2-dimethyl-1,3-dioxolan-4-yl)methyl]-6-methylquinazolin-4-amine수율 100%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8857Ethyl Acetate용매

실험 절차

A solution of 2,4-dichloro-6-methylquinazoline (300.0 mg, 1.4 mmol), triethylamine (0.5 mL) and 2,2-dimethyl-1,3-dioxolane-4-methanamine (0.2 mL, 1.5 mmol) in methanol (2.0 mL) was stirred at room temperature for 16 hours. The reaction mixture was diluted with ethyl acetate (100 mL), washed with brine (50 mL×2), dried over anhydrous sodium sulfate and then concentrated in vacuo to afford 431 mg of the crude product as a white solid. MS obsd. (ESI+) [(M+H)+] 308.

후처리

  1. washwashed with brine (50 mL×2)
  2. dry with materialdried over anhydrous sodium sulfate
  3. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-3315841718ca4bb49712ec8ca0ac19a6
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08871756B2

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