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

Chloral → 1-Methyl-alpha-trichloromethylpyrrole-2-methanol

HRID 1732560
노트
인쇄 미리보기

반응식

HRID 1732560 반응식
[OH-].[K+].[O:3]=[CH:4][C:5]([Cl:8])([Cl:7])[Cl:6].C([C:11]1[N:15]([CH3:16])[C:14](CC(OC)=O)=[CH:13][CH:12]=1)#N>O>[CH3:16][N:15]1[CH:11]=[CH:12][CH:13]=[C:14]1[CH:4]([OH:3])[C:5]([Cl:8])([Cl:7])[Cl:6]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6407ChloralHCID 14797Potassium HydroxideHCID 2386959Methyl 2-(5-cyano-1-methyl-1H-pyrrol-2-yl)acetate

생성물 1

HCID 155715331-Methyl-alpha-trichloromethylpyrrole-2-methanol

시약·촉매·용매 1

HCID 962Water용매3회

반응 조건

온도
45 °C

실험 절차

1-Methyl-2-(2',2',2'-trichloro-1'-hydroxyethyl)pyrrole (1.14 g, 5 mmol), which was prepared by the procedure of Example 2, was dissolved in the solvent (15 ml) shown in the next table. After water (15 ml) and alkali metal cyanide (MCN: amount is shown in the table) were added to the solution, a solution of potassium hydroxide in water (10 ml) was added during a period of 6 hours under vigorous stirring at 45° C. After confirmation of the disappearance of starting chloral adduct (overnight), the reaction mixture was diluted with water (100 ml) and extracted twice with ethyl acetate. The combined organic extracts were washed with brine and dried over anhydrous magnesium sulfate. Most of the solvent was removed under reduced pressure and the residue was dissolved again in the 50 ml exact amount of ethyl acetate. A portion of the solution was taken up and treated with diazomethane dissolved in ether. After removal of the excess diazomethane under reduced pressure, trans-stilbene was added as the internal standard and the yield of methyl 5-cyano-1-methylpyrrole-2-acetate (theoretical yield; 5 mmol) was determined by GC (2% EGA column, 1 m, 160° C.).

후처리

  1. additionwere added to the solution
  2. extractionextracted twice with ethyl acetate
  3. washThe combined organic extracts were washed with brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customMost of the solvent was removed under reduced pressure
  6. dissolutionthe residue was dissolved again in the 50 ml exact amount of ethyl acetate
  7. additiontreated with diazomethane
  8. dissolutiondissolved in ether
  9. customAfter removal of the excess diazomethane under reduced pressure, trans-stilbene
  10. additionwas added as the internal standard
  11. customwas determined by GC (2% EGA column, 1 m, 160° C.)

출처 및 근거

ORD 기록
ord-fbf426d271fe4d729e6d2a71ffa314ac
출처 데이터셋
uspto-grants-1980_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04238396

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트