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Sodium Methoxide → N-(3-Ethynylphenyl)-7-methoxy-6-nitroquinazolin-4-amine

HRID 1869105
ノート
印刷プレビュー

反応式

HRID 1869105 の反応式
Cl.Cl[C:3]1[CH:12]=[C:11]2[C:6]([C:7]([NH:13][C:14]3[CH:19]=[CH:18][CH:17]=[C:16]([C:20]#[CH:21])[CH:15]=3)=[N:8][CH:9]=[N:10]2)=[CH:5][C:4]=1[N+:22]([O-:24])=[O:23].[CH3:25][O-:26].[Na+]>O>[C:20]([C:16]1[CH:15]=[C:14]([NH:13][C:7]2[C:6]3[C:11](=[CH:12][C:3]([O:26][CH3:25])=[C:4]([N+:22]([O-:24])=[O:23])[CH:5]=3)[N:10]=[CH:9][N:8]=2)[CH:19]=[CH:18][CH:17]=1)#[CH:21]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 10942334Sodium MethoxideHCID 18925030HCID 18925030、化合物

生成物 1

HCID 18925009N-(3-Ethynylphenyl)-7-methoxy-6-nitroquinazolin-4-amine

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

(7-Chloro-6-nitroquinazolin-4-yl)-(3-ethynyl-phenyl)-amine hydrochloride (100 mg, 0.306 mmol and dry sodium methoxide (120 mg, 2.22 mmol) were stirred in 2 mL of dry 2-methylpyrrolidin-1-one for 8 hours at 30° C. To the cooled reaction mixture 0.93 mL of 3N and 1 mL of water were added. The mixture was diluted with 60 mL of water and extracted with two time 60 mL of ethyl acetate. The pooled organic layers were washed with three times 50 mL of water and 50 mL of brine, dried with magnesium sulfate, filtered and vacuum evaporated to afford the title product as a solid; 80 mg (82%); mp 213°-218° C. dec.

後処理

  1. additionwere added
  2. extractionextracted with two time 60 mL of ethyl acetate
  3. washThe pooled organic layers were washed with three times 50 mL of water and 50 mL of brine
  4. dry with materialdried with magnesium sulfate
  5. filtrationfiltered
  6. customvacuum evaporated

出典と根拠

ORDレコード
ord-f75bca94dc0b418caff7bd5b267f5ef9
出典データセット
uspto-grants-2009_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
USRE041065E1

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート