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

Triethylamine → HCID 178503239, 화합물

HRID 609536
노트
인쇄 미리보기

반응식

HRID 609536 반응식
I[C:2]1[CH:7]=[CH:6][C:5]([C:8]([F:11])([F:10])[F:9])=[CH:4][C:3]=1[S:12][CH3:13].[CH:14]1([C:17]2[CH:21]=[C:20]([OH:22])[N:19]([CH3:23])[N:18]=2)[CH2:16][CH2:15]1.C(N(CC)CC)C.[C:31](=O)([O-])[O-:32].[K+].[K+]>O1CCOCC1>[CH:14]1([C:17]2[C:21]([C:31](=[O:32])[C:2]3[CH:7]=[CH:6][C:5]([C:8]([F:11])([F:10])[F:9])=[CH:4][C:3]=3[S:12][CH3:13])=[C:20]([OH:22])[N:19]([CH3:23])[N:18]=2)[CH2:16][CH2:15]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 11430Potassium CarbonateHCID 19599111(2-Iodo-5-(trifluoromethyl)phenyl)(methyl)sulfaneHCID 178481725HCID 178481725, 화합물

생성물 1

HCID 178503239HCID 178503239, 화합물수율 89.3%

시약·촉매·용매 1

HCID 312751,4-Dioxane
용매

실험 절차

Into a 200 ml autoclave, 1.59 g of 4-iodo-3-methylthiobenzotrifluoride prepared in accordance with the following Preparation Example 10, 1.38 g of 3-cyclopropyl-5-hydroxy-1-methylpyrazole (after-mentioned Intermediate No. 1a-1), 0.5 g of triethylamine, 3.1 g of potassium carbonate, 0.22 g of palladium (II) bis-triphenylphosphine) dichloride and 40 ml of dioxane were put and sealed, and the interior of the autoclave was flushed with carbon monoxide (pressure: 65 kg/cm2), followed by a reaction at 140° C. for 8 hours. After completion of the reaction, the solvent was distilled off, and the residue was dissolved in water, and then insoluble matters were filtered off. The filtrate was washed with dichloromethane. The washed product was acidified (pH=1) with concentrated hydrochloric acid and extracted with dichloromethane. The obtained extract solution was dried over anhydrous sodium sulfate, and the solvent was distilled off to obtain 1.59 g of 3-cyclopropyl-1-methyl-4-(2-methylthio-4-trifluoromethylbenzoyl)-5-hydroxypyrazole (after-mentioned Compound No. a-82) as a reddish brown solid.

후처리

  1. customsealed
  2. customthe interior of the autoclave was flushed with carbon monoxide (pressure: 65 kg/cm2)
  3. customfollowed by a reaction at 140° C. for 8 hours
  4. customAfter completion of the reaction
  5. distillationthe solvent was distilled off
  6. dissolutionthe residue was dissolved in water
  7. filtrationinsoluble matters were filtered off
  8. washThe filtrate was washed with dichloromethane
  9. extractionextracted with dichloromethane
  10. extractionThe obtained extract solution
  11. dry with materialwas dried over anhydrous sodium sulfate
  12. distillationthe solvent was distilled off

출처 및 근거

ORD 기록
ord-8b46b6be1f6048e5a957e711e89a2524
출처 데이터셋
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05998334

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트