HCID 178441857、化合物 → HCID 178441854、化合物

HRID 487058ノート

反応式

HRID 487058 の反応式
[CH2:1]([C:5]1[NH:6][C:7]2[C:12]([C:13](=[O:15])[N:14]=1)=[CH:11][C:10]([CH:16]=[O:17])=[CH:9][CH:8]=2)[CH2:2][CH2:3][CH3:4].[C:18]1([Li])[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1>O1CCCC1>[CH2:1]([C:5]1[NH:6][C:7]2[C:12]([C:13](=[O:15])[N:14]=1)=[CH:11][C:10]([CH:16]([OH:17])[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)=[CH:9][CH:8]=2)[CH2:2][CH2:3][CH3:4]

参加物

4

反応物 2

HCID 178441857HCID 178441857、化合物HCID 178506676HCID 178506676、化合物

生成物 1

HCID 178441854HCID 178441854、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a stirred solution of 2.00 g of 2-butyl-1,4-dihydro-4-oxo-6-quinazolinecarboxaldehyde in 100 ml of tetrahydrofuran, cooled at 0° C., is added 13.0 ml of 2.0M phenyllithium and stirring continued is for 1 hour. The cooling is removed and the reaction allowed to reach room-temperature followed by an additional 30 minutes at room temperature. The reaction is diluted with saturated ammonium chloride solution and extracted with ethyl acetate. The organic layer is dried, evaporated to a residue, which is purified by chromatography on silica gel by elution with 0.25:100 methanol-chloroform to give 0.932 g of the desired product.

後処理

  1. customThe cooling is removed
  2. waitfollowed by an additional 30 minutes at room temperature
  3. additionThe reaction is diluted with saturated ammonium chloride solution
  4. extractionextracted with ethyl acetate
  5. customThe organic layer is dried
  6. customevaporated to a residue, which
  7. customis purified by chromatography on silica gel by elution with 0.25:100 methanol-chloroform

出典と根拠

ORDレコード
ord-04d2c50aa10845d8a77e85ba65eaa0f4
出典データセット
uspto-grants-1994_03
特許番号
US05294611

反応ノート

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