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

Toluene → 3-[3-(3,6-Dihydro-4,6,6-trimethyl-2H-pyran-2-yl)-1,2-benzisothiazol-5-yl]-1-methyl-6-(trifluoromethyl)uracil

HRID 49010
노트
인쇄 미리보기

반응식

HRID 49010 반응식
[CH3:1][N:2]1[C:7]([C:8]([F:11])([F:10])[F:9])=[CH:6][C:5](=[O:12])[N:4]([C:13]2[CH:14]=[CH:15][C:16]3[S:20][N:19]=[C:18]([CH:21]=[O:22])[C:17]=3[CH:23]=2)[C:3]1=[O:24].[CH3:25][C:26](O)([CH2:28][C:29]([CH3:32])(O)[CH3:30])[CH3:27].C1(C)C=CC(S(O)(=O)=O)=CC=1.C1(C)C=CC=CC=1>C(OCC)C.C(OCC)(=O)C.O>[CH3:25][C:26]1[CH2:27][CH:21]([C:18]2[C:17]3[CH:23]=[C:13]([N:4]4[C:5](=[O:12])[CH:6]=[C:7]([C:8]([F:9])([F:10])[F:11])[N:2]([CH3:1])[C:3]4=[O:24])[CH:14]=[CH:15][C:16]=3[S:20][N:19]=2)[O:22][C:29]([CH3:32])([CH3:30])[CH:28]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 1140TolueneHCID 6101p-Toluenesulfonic acidHCID 1411532,4-Pentanediol, 2,4-dimethyl-HCID 178523685-[3,6-dihydro-3-methyl-2,6-dioxo-4-(trifluoromethyl)-1(2H)-pyrimidinyl]-1, 2-benzisothiazole-3-carboxaldehyde

생성물 1

HCID 206342123-[3-(3,6-Dihydro-4,6,6-trimethyl-2H-pyran-2-yl)-1,2-benzisothiazol-5-yl]-1-methyl-6-(trifluoromethyl)uracil수율 31.4%

시약·촉매·용매 3

HCID 962Water용매HCID 3283Diethyl Ether용매HCID 8857Ethyl Acetate용매

실험 절차

A mixture of 5-[3,6-dihydro-3-methyl-2,6-dioxo-4-(trifluoromethyl)-1(2H)-pyrimidinyl]-1, 2-benzisothiazole-3-carboxaldehyde(0.500 g, 0.00141 mol), 2,4-dimethyl-2,4-pentanediol (0.260 g, 0.00183 mol), p-toluenesulfonic acid (0.0100 g, 0.000071 mol) and toluene is stirred overnight at reflux with azeotropic removal of water. The mixture is cooled to room temperature, diluted with diethyl ether and ethyl acetate and washed with two prortions of water and brine. The organic layer is dried and concentrated in vacuo to a brown oil, which is chromatographed on silica gel with ethyl acetate-hexanes to afford the title compound as a white solid (0.200 g, 31.4%, mp 88-92° C.) which is characterized by NMR spectral analysis.

후처리

  1. washwashed with two prortions of water and brine
  2. customThe organic layer is dried
  3. concentrationconcentrated in vacuo to a brown oil, which
  4. customis chromatographed on silica gel with ethyl acetate-hexanes

출처 및 근거

ORD 기록
ord-ca22450bb37740998ec0ebe68c4f1155
출처 데이터셋
uspto-grants-2004_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06706663B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트