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

Methyl vinyl ketone → (3E)-4-[2-(4-isopropoxyphenoxy)-1,3-thiazol-5-yl]but-3-en-2-one

HRID 2078450
노트
인쇄 미리보기

반응식

HRID 2078450 반응식
I[C:2]1[S:6][C:5]([O:7][C:8]2[CH:13]=[CH:12][C:11]([O:14][CH:15]([CH3:17])[CH3:16])=[CH:10][CH:9]=2)=[N:4][CH:3]=1.C(N(CC)CC)C.[CH3:25][C:26]([CH:28]=[CH2:29])=[O:27]>CN(C)C=O.[Cl-].C([N+](CCCC)(CCCC)CCCC)CCC.C(OCC)(=O)C.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>[CH:15]([O:14][C:11]1[CH:12]=[CH:13][C:8]([O:7][C:5]2[S:6][C:2](/[CH:29]=[CH:28]/[C:26](=[O:27])[CH3:25])=[CH:3][N:4]=2)=[CH:9][CH:10]=1)([CH3:17])[CH3:16]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 3

HCID 6570Methyl vinyl ketoneHCID 8471TriethylamineHCID 67097044HCID 67097044, 화합물

생성물 1

HCID 67096854(3E)-4-[2-(4-isopropoxyphenoxy)-1,3-thiazol-5-yl]but-3-en-2-one수율 85.6%

시약·촉매·용매 4

HCID 70681Tetrabutylammonium Chloride촉매
HCID 178418476
HCID 178418476, 화합물
촉매
HCID 6228Dimethylformamide용매
HCID 8857Ethyl Acetate용매

반응 조건

온도
75 °C

실험 절차

To a solution of the product from Example 7B (1.6 g, 4.43 mmole) in N,N-dimethylformamide (25 mL) was consecutively added triethylamine (8 mL), tetrabutyl ammonium chloride (1.2 g, 4.3 mmole), methylvinylketone (2 g, 28.5 mmole) and dichlorobis(triphenylphosphine)palladium(II) (155 mg, 0.22 mmole). The reaction mixture was heated at 75° C. overnight. The reaction mixture was diluted with ethyl acetate and washed with 0.5N aqueous HCl, followed by brine. The reaction mixture was dried over magnesium sulfate filtered and evaporated. The product was purified via silica column, using a gradient of 5-25% ethyl acetate in hexane, to yield 1.15 g (85%) of orange solid. 1H NMR (300 MHz, CDCl3) δ ppm 7.50 (d, J=15.44 Hz, 1H) 7.42 (s, 1H) 7.13-7.24 (m, 2 H) 6.84-7.00 (m, 2H) 6.23 (d, J=15.81 Hz, 1H) 4.38-4.63 (m, 1H) 2.30 (s, 3H) 1.35 (t, J=5.52 Hz, 6H). Mass spectrum DCI 304 (M+H)+.

후처리

  1. washwashed with 0.5N aqueous HCl
  2. dry with materialThe reaction mixture was dried over magnesium sulfate
  3. filtrationfiltered
  4. customevaporated
  5. customThe product was purified via silica column

출처 및 근거

ORD 기록
ord-6ff95b0b1cc64805a880f211cde9b128
출처 데이터셋
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07928243B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트