2-Butyl-1,2-dihydro-4-oxo-6-quinazolinecarboxaldehyde → HCID 178441854, 화합물

HRID 1974933노트

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HRID 1974933 반응식
[CH2:1]([CH:5]1[NH:14][C:13](=[O:15])[C:12]2[C:7](=[CH:8][CH:9]=[C:10]([CH:16]=[O:17])[CH:11]=2)[NH:6]1)[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]

참가 물질

4

반응물 2

HCID 191008472-Butyl-1,2-dihydro-4-oxo-6-quinazolinecarboxaldehydeHCID 178506676HCID 178506676, 화합물

생성물 1

HCID 178441854HCID 178441854, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a stirred solution of 2.00 g of 2-butyl-1,2-dihydro-4-oxo-6-quinazolinecarboxaldehyde in 100 ml of tetrahydrofuran, cooled at 0° C., is added 13.0 ml of 2.0 M phenyllithium and stirring continued 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. CI MASS SPEC 309(MH+).

후처리

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

출처 및 근거

ORD 기록
ord-4fa1ee90765d4242bee4c6959aee9883
출처 데이터셋
uspto-grants-1994_02
특허 번호
US05284852

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