HCID 2794448, 화합물 → HCID 21257365, 화합물

HRID 636073노트

반응식

HRID 636073 반응식
C[O:2][C:3]1[CH:12]=[C:11]([O:13]C)[CH:10]=[C:9]2[C:4]=1[C:5]([CH3:16])=[CH:6][C:7](=[O:15])[NH:8]2.[Cl-].[Al+3].[Cl-].[Cl-].C(Cl)(Cl)Cl.CO>ClC1C=CC=CC=1>[OH:2][C:3]1[CH:12]=[C:11]([OH:13])[CH:10]=[C:9]2[C:4]=1[C:5]([CH3:16])=[CH:6][C:7](=[O:15])[NH:8]2

참가 물질

5

반응물 3

HCID 2794448HCID 2794448, 화합물HCID 6451240Aluminum(III) ChlorideHCID 21584188Chloroform methanol

생성물 1

HCID 21257365HCID 21257365, 화합물수율 96.2%

시약·촉매·용매 1

HCID 7964Chlorobenzene용매

실험 절차

To a stirred solution of compound 11 (12.5 g, 57.07 mmol) in chlorobenzene (100 mL), aluminium chloride (37 g, 285.3 mmol) was added in portions over a period of 10 min and heated at 100° C. overnight (TLC chloroform: methanol 9:1, Rf=0.2). The reaction mixture was then cooled to room temperature, poured on crushed ice (300 g) and stirred well for 30 min. The solid separated was filtered washed with water till neutral to pH. It was then washed with hexane (50 mL) and dried to give product 5,7-dihydroxy-4-methyl-1,2-dihydro-2-quinolinone (13, 10.5 g) in 96% yield as a dark brown solid. M.P. >300° C.

후처리

  1. additionpoured
  2. customThe solid separated
  3. filtrationwas filtered
  4. washwashed with water till neutral
  5. washIt was then washed with hexane (50 mL)
  6. customdried

출처 및 근거

ORD 기록
ord-86af25b5c5fc447892498fb032a94565
출처 데이터셋
uspto-grants-2001_02
특허 번호
US06191279B1

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