Water → HCID 12851825, 화합물

HRID 1156898노트

반응식

HRID 1156898 반응식
[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

참가 물질

7

반응물 4

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

생성물 1

HCID 12851825HCID 12851825, 화합물수율 44.3%

시약·촉매·용매 2

HCID 7237O-Xylene용매HCID 24813Phosphorus oxychloride용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7719e64ba9a14481bd262f072a3001eb
출처 데이터셋
uspto-grants-1982_06
특허 번호
US04337256

반응 노트

불러오는 중…