홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Phosphorus oxide (P4O10) → HCID 59396590, 화합물

HRID 2383031
노트
인쇄 미리보기

반응식

HRID 2383031 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([CH2:9][CH2:10][NH:11][C:12]([CH:14]2[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]2)=O)=[CH:5][CH:4]=1.O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O.P(Cl)(Cl)(Cl)=O>C1(C)C=CC=CC=1>[CH:14]1([C:12]2[C:7]3[C:6](=[CH:5][CH:4]=[C:3]([O:2][CH3:1])[CH:8]=3)[CH2:9][CH2:10][N:11]=2)[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 14812Phosphorus oxide (P4O10)HCID 24813Phosphorus oxychlorideHCID 874953HCID 874953, 화합물

생성물 1

HCID 59396590HCID 59396590, 화합물수율 36.1%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

N-[2-(4-methoxyphenyl)ethyl]cyclohexanecarboxamide (5.56 g) was dissolved in toluene (120 mL), and diphosphorus pentoxide (3.0 g) and phosphorus oxychloride (6.0 mL) were sequentially added thereto, followed by stirring under heating at reflux for 5.5 hours. The reaction mixture was left to cool and then the solvent was evaporated. An aqueous 8 M potassium hydroxide solution, water and chloroform were added to the resulting residue to completely dissolve the insoluble materials to achieve a pH of around pH 8, followed by extraction with chloroform. The extract was washed with saturated brine, and then dried over magnesium sulfate. The solvent was evaporated and the resulting residue was purified by silica gel column chromatography (chloroform-MeOH) to obtain 1-cyclohexyl-7-methoxy-3,4-dihydroisoquinoline (1.87 g).

후처리

  1. temperatureunder heating
  2. temperatureat reflux for 5.5 hours
  3. waitThe reaction mixture was left
  4. temperatureto cool
  5. customthe solvent was evaporated
  6. additionAn aqueous 8 M potassium hydroxide solution, water and chloroform were added to the resulting residue
  7. dissolutionto completely dissolve the insoluble materials
  8. extractionfollowed by extraction with chloroform
  9. washThe extract was washed with saturated brine
  10. dry with materialdried over magnesium sulfate
  11. customThe solvent was evaporated
  12. customthe resulting residue was purified by silica gel column chromatography (chloroform-MeOH)

출처 및 근거

ORD 기록
ord-3405bd4f47734d88aa64dfb986177f78
출처 데이터셋
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08263607B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트