Ethyl bromoacetate → Ethyl {3-[(4-bromo-2-fluorophenyl)methyl]-7-chloro-2,4-dioxo-3,4-dihydroquinazolin-1(2H)-yl}acetate

HRID 1639312

反応式

HRID 1639312 の反応式
[Br:1][C:2]1[CH:21]=[CH:20][C:5]([CH2:6][N:7]2[C:16](=[O:17])[C:15]3[C:10](=[CH:11][C:12]([Cl:18])=[CH:13][CH:14]=3)[NH:9][C:8]2=[O:19])=[C:4]([F:22])[CH:3]=1.Br[CH2:24][C:25]([O:27][CH2:28][CH3:29])=[O:26].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[Br:1][C:2]1[CH:21]=[CH:20][C:5]([CH2:6][N:7]2[C:16](=[O:17])[C:15]3[C:10](=[CH:11][C:12]([Cl:18])=[CH:13][CH:14]=3)[N:9]([CH2:24][C:25]([O:27][CH2:28][CH3:29])=[O:26])[C:8]2=[O:19])=[C:4]([F:22])[CH:3]=1

参加物

5

反応物 3

HCID 7748Ethyl bromoacetateHCID 11430Potassium CarbonateHCID 144237993-(4-bromo-2-fluorobenzyl)-7-chloro-2,4(1H,3H)-quinazolinedione

生成物 1

HCID 11431340Ethyl {3-[(4-bromo-2-fluorophenyl)methyl]-7-chloro-2,4-dioxo-3,4-dihydroquinazolin-1(2H)-yl}acetate収率 89.8%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of 3-(4-bromo-2-fluorobenzyl)-7-chloro-1,2,3,4-tetrahydro-2,4-dioxoquinazoline (500 mg), ethyl bromoacetate (218 mg) and potassium carbonate (360 mg) in N,N-dimethylformamide (5 ml) was stirred at 30° C. for 30 minutes. The solution was evaporated and the residue was dissolved in ethyl acetate. The solution was washed in turn with 0.5N aqueous hydrochloric acid and water, and then dried over magnesium sulfate. The solvent was removed in vacuo to give a crystalline residue, which was crystallized from a mixture of ethyl acetate and n-hexane to give ethyl 2-[3-(4-bromo-2-fluorobenzyl)-7-chloro-1,2,3,4-tetrahydro-2,4-dioxoquinazolin-1-yl]acetate (550 mg).

後処理

  1. customThe solution was evaporated
  2. dissolutionthe residue was dissolved in ethyl acetate
  3. washThe solution was washed in turn with 0.5N aqueous hydrochloric acid and water
  4. dry with materialdried over magnesium sulfate
  5. customThe solvent was removed in vacuo
  6. customto give a crystalline residue, which
  7. customwas crystallized from a mixture of ethyl acetate and n-hexane

出典と根拠

ORDレコード
ord-da1caf00f70f43c8b47dc88d6a12ba1e
出典データセット
uspto-grants-1989_11
特許番号
US04883800

関連ノート

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