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

Iodoethane → HCID 12813183, 화합물

HRID 1154983
노트
인쇄 미리보기

반응식

HRID 1154983 반응식
[F:1][C:2]([F:26])([F:25])[C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([N:9]2[C:13](=[O:14])[C:12]([C:15]3[CH:16]=[C:17]([C:21]([F:24])([F:23])[F:22])[CH:18]=[CH:19][CH:20]=3)=[CH:11][NH:10]2)[CH:4]=1.[CH2:27](I)[CH3:28].C(=O)([O-])[O-].[K+].[K+]>C(O)C>[F:26][C:2]([F:1])([F:25])[C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([N:9]2[C:13](=[O:14])[C:12]([C:15]3[CH:16]=[C:17]([C:21]([F:22])([F:23])[F:24])[CH:18]=[CH:19][CH:20]=3)=[CH:11][N:10]2[CH2:27][CH3:28])[CH:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6340IodoethaneHCID 11430Potassium CarbonateHCID 12813180HCID 12813180, 화합물

생성물 1

HCID 12813183HCID 12813183, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A 4 gram portion of 1,4-bis-(α,α,α-trifluoro-3-tolyl)-3-pyrazolin-5-one (from Example 4) was heated with 20 ml. ethyl iodide, 3 grams potassium carbonate, and 40 ml. ethanol at reflux temperature for about 4 hours. The reaction product mixture was concentrated in vacuo and extracted with ethyl acetate. The extract was dried over anhydrous magnesium sulfate, the drying agent filtered off and the filtrate concentrated in vacuo. On standing overnight the residue solidified and was recrystallized from a mixture of hexane and benzene. The solid was chromatographed on a silica gel column using a mixture of ethyl acetate and hexane in the ratio of 1:2. The product from the column was then recrystallized from a mixture of hexane and benzene to yield the desired product, m.p. 110°-111° C.

후처리

  1. concentrationThe reaction product mixture was concentrated in vacuo
  2. extractionextracted with ethyl acetate
  3. dry with materialThe extract was dried over anhydrous magnesium sulfate
  4. filtrationthe drying agent filtered off
  5. concentrationthe filtrate concentrated in vacuo
  6. customthe residue solidified and was recrystallized from a mixture of hexane and benzene
  7. customThe solid was chromatographed on a silica gel column
  8. additiona mixture of ethyl acetate and hexane in the ratio of 1:2
  9. customThe product from the column was then recrystallized from a mixture of hexane and benzene

출처 및 근거

ORD 기록
ord-889d6887f20e400288a44421f9d116f9
출처 데이터셋
uspto-grants-1981_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04299614

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트