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Sodium Hydroxide → 4-(((1,2-Dihydro-3-methyl-1-oxobenzo(f)quinazolin-9-yl)methyl)amino)-2-fluorobenzoic acid

HRID 369776
ノート
印刷プレビュー

反応式

HRID 369776 の反応式
[CH3:1][C:2]1[NH:11][C:10](=[O:12])[C:9]2[C:8]3[CH:13]=[C:14]([CH2:17][NH:18][C:19]4[CH:29]=[CH:28][C:22]([C:23]([O:25]CC)=[O:24])=[C:21]([F:30])[CH:20]=4)[CH:15]=[CH:16][C:7]=3[CH:6]=[CH:5][C:4]=2[N:3]=1.[OH-].[Na+]>CCO>[CH3:1][C:2]1[NH:11][C:10](=[O:12])[C:9]2[C:8]3[CH:13]=[C:14]([CH2:17][NH:18][C:19]4[CH:29]=[CH:28][C:22]([C:23]([OH:25])=[O:24])=[C:21]([F:30])[CH:20]=4)[CH:15]=[CH:16][C:7]=3[CH:6]=[CH:5][C:4]=2[N:3]=1
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 14798Sodium HydroxideHCID 135708790HCID 135708790、化合物

生成物 1

HCID 1357087934-(((1,2-Dihydro-3-methyl-1-oxobenzo(f)quinazolin-9-yl)methyl)amino)-2-fluorobenzoic acid収率 80.6%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A 100 mL 3-necked flask equipped with a magnetic stirrer was charged with 0.200 g of ethyl 4-(((1,2-dihydro-3-methyl-1-oxobenzo(f)quinazolin-9-yl)methyl)amino)-2-fluorobenzoate, 18 mL of 1 N NaOH, and 20 mL of EtOH. After stirring overnight at RT, the solution was concentrated to 20 mL in vacuo and acidified to pH 2.5 by addition of concentrated HCl. The resulting precipitate was collected by vacuum filtration, washed with 15 mL of water, and dried in vacuo to afford 0.15 g (77%) of 4-(((1,2-dihydro-3-methyl-1-oxobenzo(f)quinazolin-9-yl)methyl)amino)-2-fluorobenzoic acid as a white powder, m.p. >250° C.

後処理

  1. customA 100 mL 3-necked flask equipped with a magnetic stirrer
  2. concentrationthe solution was concentrated to 20 mL in vacuo
  3. additionacidified to pH 2.5 by addition of concentrated HCl
  4. filtrationThe resulting precipitate was collected by vacuum filtration
  5. washwashed with 15 mL of water
  6. customdried in vacuo

出典と根拠

ORDレコード
ord-77084ecb8a814669b28a626396d26cad
出典データセット
uspto-grants-2000_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06140100

反応ノート

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