HCID 178441857, 화합물 → HCID 178441854, 화합물

HRID 487058노트

반응식

HRID 487058 반응식
[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]

참가 물질

4

반응물 2

HCID 178441857HCID 178441857, 화합물HCID 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-1,4-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.

후처리

  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

출처 및 근거

ORD 기록
ord-04d2c50aa10845d8a77e85ba65eaa0f4
출처 데이터셋
uspto-grants-1994_03
특허 번호
US05294611

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