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

HRID 540252ノート

反応式

HRID 540252 の反応式
[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

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-3315841718ca4bb49712ec8ca0ac19a6
出典データセット
uspto-grants-2014_10
特許番号
US08871756B2

反応ノート

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