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Water → 2-[3-(2-Chlorophenyl)-6-fluoro-4-oxo-3,4-dihydroquinazolin-2-yl-vinyl)pyridine-2-carbaldehyde

HRID 843648
ノート
印刷プレビュー

反応式

HRID 843648 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N:8]1[C:17](=[O:18])[C:16]2[C:11](=[CH:12][CH:13]=[C:14]([F:19])[CH:15]=2)[N:10]=[C:9]1[CH3:20].[N:21]1[C:26]([CH:27]=[O:28])=[CH:25][CH:24]=[CH:23][C:22]=1C=O.O.O1CCOC[CH2:33]1>C(OC(=O)C)(=O)C.[Cl-].[Zn+2].[Cl-]>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N:8]1[C:17](=[O:18])[C:16]2[C:11](=[CH:12][CH:13]=[C:14]([F:19])[CH:15]=2)[N:10]=[C:9]1[CH:20]=[CH:33][C:26]1([CH:27]=[O:28])[CH:25]=[CH:24][CH:23]=[CH:22][NH:21]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 962WaterHCID 312751,4-DioxaneHCID 640654(3H)-Quinazolinone, 3-(2-chlorophenyl)-6-fluoro-2-methyl-HCID 794852,6-Diformylpyridine

生成物 1

HCID 865838672-[3-(2-Chlorophenyl)-6-fluoro-4-oxo-3,4-dihydroquinazolin-2-yl-vinyl)pyridine-2-carbaldehyde

試薬・触媒・溶媒 2

HCID 3007855
Zincchloride
触媒
HCID 7918Acetic Anhydride溶媒

実験手順

A catalytic amount (about 100 mg) of anhydrous zinc chloride was added to a solution of 576 mg (2.0 mmol) of 3-(2-chlorophenyl)-6-fluoro-2-methyl-4(3H)-quinazolinone and 270 mg (2.0 mmol) of 2,6-pyridinedicarboxaldehyde in 20-25 mL of dioxane and 1.0 mL of acetic anhydride. The reaction mixture was heated at reflux under a nitrogen atmosphere for 3 hours until TLC indicated that the starting materials had been consumed. The cooled reaction mixture was poured into water and the mixture was extracted with ethyl acetate. The combined extracts were dried with brine and magnesium sulfate, treated with decolonizing carbon and filtered and the solvent was removed to give the desired product. This was taken up in 2:1 ether/pentane and the crystals were filtered to give 266 mg of the product, 33%, m.p. 247-248° C.

後処理

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux under a nitrogen atmosphere for 3 hours until TLC
  3. customhad been consumed
  4. customThe cooled reaction mixture
  5. extractionthe mixture was extracted with ethyl acetate
  6. dry with materialThe combined extracts were dried with brine and magnesium sulfate
  7. additiontreated with decolonizing carbon
  8. filtrationfiltered
  9. customthe solvent was removed

出典と根拠

ORDレコード
ord-e414f10c31ef4c24873d9551f513cbb0
出典データセット
uspto-grants-2002_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06380204B1

反応ノート

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