Water → HCID 12851825、化合物

HRID 1156898ノート

反応式

HRID 1156898 の反応式
[C:1]1([CH3:19])[CH:6]=[CH:5][C:4]([C:7]([NH:9][CH2:10][CH2:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=2[Cl:18])=O)=[CH:3][CH:2]=1.O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O.O.[OH-].[Na+]>C1(C)C(C)=CC=CC=1.P(Cl)(Cl)(Cl)=O>[CH3:19][C:1]1[CH:6]=[CH:5][C:4]([C:7]2[C:17]3[C:12](=[C:13]([Cl:18])[CH:14]=[CH:15][CH:16]=3)[CH2:11][CH2:10][N:9]=2)=[CH:3][CH:2]=1

参加物

7

反応物 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 14812Phosphorus oxide (P4O10)HCID 128518181-(p-Toluoylamino)-2-(2-chlorophenyl)ethane

生成物 1

HCID 12851825HCID 12851825、化合物収率 44.3%

試薬・触媒・溶媒 2

HCID 7237O-Xylene溶媒HCID 24813Phosphorus oxychloride溶媒

実験手順

1-(p-Toluoylamino)-2-(2-chlorophenyl)ethane (70 g) was dissolved in 700 ml of xylene and 320 ml of phosphorus oxychloride, and while the solution was heated with stirring, 240 g of phosphorus pentoxide was added. The mixture was heated under reflux for 4 hours. Water was added to the reaction mixture. The aqueous layer was made weakly alkaline with an aqueous solution of sodium hydroxide, extracted with benzene, washed in water, and dried. The solvent was distilled off, and the residue was recrystallized from benzene to afford 29 g of 1-(4-methylphenyl)-5-chloro-3,4-dihydroisoquinoline as colorless needles.

後処理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 4 hours
  3. extractionextracted with benzene
  4. washwashed in water
  5. customdried
  6. distillationThe solvent was distilled off
  7. customthe residue was recrystallized from benzene

出典と根拠

ORDレコード
ord-7719e64ba9a14481bd262f072a3001eb
出典データセット
uspto-grants-1982_06
特許番号
US04337256

反応ノート

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