Phosphorus oxide (P4O10) → HCID 12851821, 화합물

HRID 1156868노트

반응식

HRID 1156868 반응식
[Br:1][C:2]1[CH:19]=[CH:18][C:5]([C:6]([NH:8][CH2:9][CH2:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[CH3:17])=O)=[CH:4][CH:3]=1.P(Cl)(Cl)(Cl)=O.O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O>C1(C)C(C)=CC=CC=1>[Br:1][C:2]1[CH:19]=[CH:18][C:5]([C:6]2[C:16]3[C:11](=[C:12]([CH3:17])[CH:13]=[CH:14][CH:15]=3)[CH2:10][CH2:9][N:8]=2)=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 14812Phosphorus oxide (P4O10)HCID 24813Phosphorus oxychlorideHCID 128518091-(4-Bromobenzoylamino)-2-(2-methylphenyl)ethane

생성물 1

HCID 12851821HCID 12851821, 화합물

시약·촉매·용매 1

HCID 7237O-Xylene용매

실험 절차

Forty-four (44) grams of 1-(4-bromobenzoylamino)-2-(2-methylphenyl)ethane was heated with stirring at 140° C. for 4 hours together with 300 ml of xylene, 100 ml of phosphorus oxychloride and 100 g of phosphorus pentoxide. The reaction mixture was decanted to remove the solvent. The residue was carefully decomposed with ice water, and made weakly alkaline with an aqueous solution of sodium hydroxide. The crystals precipitated were extracted with benzene, and dried, followed by distilling off the solvent. Recrystallization of the residue from hexane afforded 35 g of 1-(4-bromophenyl)-5-methyl-3,4-dihydroisoquinoline as colorless needles having a melting point of 60.0° to 61.5° C.

후처리

  1. customThe reaction mixture was decanted
  2. customto remove the solvent
  3. customThe crystals precipitated
  4. extractionwere extracted with benzene
  5. customdried
  6. distillationby distilling off the solvent
  7. customRecrystallization of the residue from hexane

출처 및 근거

ORD 기록
ord-4a5359cb006448359935601ed1a06d2b
출처 데이터셋
uspto-grants-1982_06
특허 번호
US04337256

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