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

Triethylamine → HCID 12813178, 화합물

HRID 1154979
노트
인쇄 미리보기

반응식

HRID 1154979 반응식
C[N:2]1[CH:6]=[C:5]([C:7]2[CH:8]=[C:9]([C:13]([F:16])([F:15])[F:14])[CH:10]=[CH:11][CH:12]=2)[C:4](=[O:17])[N:3]1[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.Cl.[Cl:25]C1C=C(NN)C=CC=1.C(N(CC)CC)C>C1(C)C=CC=C(C)C=1>[Cl:25][C:20]1[CH:19]=[C:18]([N:3]2[C:4](=[O:17])[C:5]([C:7]3[CH:8]=[C:9]([C:13]([F:16])([F:15])[F:14])[CH:10]=[CH:11][CH:12]=3)=[CH:6][NH:2]2)[CH:23]=[CH:22][CH:21]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 75331m-Chlorophenylhydrazine hydrochlorideHCID 128131761,2-Dihydro-1-methyl-2-phenyl-4-[3-(trifluoromethyl)phenyl]-3H-pyrazol-3-one

생성물 1

HCID 12813178HCID 12813178, 화합물

시약·촉매·용매 1

HCID 7929M-Xylene용매

실험 절차

A 3.5 gram portion of the atropic ester of Example 1 was reacted with 2.3 grams 3-chlorophenylhydrazine hydrochloride in the presence of 1.3 grams triethylamine in about 50 ml. meta-xylene. The mixture was then stirred at reflux overnight, and the reaction mixture evaporated to dryness under vacuum. The residue was partitioned between ethyl acetate and water, and the organic layer was dried over sodium sulfate and evaporated to dryness. The residue was chromatographed on silica gel with ethyl acetate as the eluant. The product containing fractions were combined and evaporated to dryness to produce a crude product, which was recrystallized from methanol to produce 2 grams 1-(3-chlorophenyl)-4-(α,α,α-trifluoro-3-tolyl)-3-pyrazolin-5-one, m.p. 182°-184° C.

후처리

  1. temperatureat reflux overnight
  2. customthe reaction mixture evaporated to dryness under vacuum
  3. customThe residue was partitioned between ethyl acetate and water
  4. dry with materialthe organic layer was dried over sodium sulfate
  5. customevaporated to dryness
  6. customThe residue was chromatographed on silica gel with ethyl acetate as the eluant
  7. additionThe product containing fractions
  8. customevaporated to dryness
  9. customto produce a crude product, which
  10. customwas recrystallized from methanol

출처 및 근거

ORD 기록
ord-209559267bdf4e16842776d17528a7d2
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