HCID 2794448、化合物 → HCID 21257365、化合物

HRID 636073ノート

反応式

HRID 636073 の反応式
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

参加物

5

反応物 3

HCID 2794448HCID 2794448、化合物HCID 6451240Aluminum(III) ChlorideHCID 21584188Chloroform methanol

生成物 1

HCID 21257365HCID 21257365、化合物収率 96.2%

試薬・触媒・溶媒 1

HCID 7964Chlorobenzene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-86af25b5c5fc447892498fb032a94565
出典データセット
uspto-grants-2001_02
特許番号
US06191279B1

反応ノート

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