5,6-Dinitro-2-(2,2,2-trifluoroethyl)-2-(trifluoromethyl)-1,3-benzodioxole → HCID 53895814, 화합물

HRID 37581노트

반응식

HRID 37581 반응식
[N+:1]([C:4]1[C:21]([N+:22]([O-])=O)=[CH:20][C:7]2[O:8][C:9]([CH2:15][C:16]([F:19])([F:18])[F:17])([C:11]([F:14])([F:13])[F:12])[O:10][C:6]=2[CH:5]=1)([O-])=O.[H][H]>O1CCCC1>[NH2:22][C:21]1[C:4]([NH2:1])=[CH:5][C:6]2[O:10][C:9]([CH2:15][C:16]([F:19])([F:18])[F:17])([C:11]([F:12])([F:13])[F:14])[O:8][C:7]=2[CH:20]=1

참가 물질

4

반응물 2

HCID 536607065,6-Dinitro-2-(2,2,2-trifluoroethyl)-2-(trifluoromethyl)-1,3-benzodioxoleHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 53895814HCID 53895814, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

39 g of the product of Example 29 were dissolved in 2000 ml of tetrahydrofuran, and 20 g of catalyst (palladium-on-charcoal, 5% by weight) were added. The reaction mixture was hydrogenated with hydrogen at 25 to 30 bar for 13 hours at room temperature. It was then filtered and the solvent was stripped off under vacuum to leave a solid. The yield was 274 g (=96% of theory). 19F NMR: -61.2 and -86.6 ppm. 1H NMR: 3.02 ppm.

후처리

  1. filtrationIt was then filtered
  2. customto leave a solid

출처 및 근거

ORD 기록
ord-dccbff797dcf4cf2a342bdcee39e6638
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05420309

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