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

HRID 37581ノート

反応式

HRID 37581 の反応式
[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

参加物

4

反応物 2

HCID 536607065,6-Dinitro-2-(2,2,2-trifluoroethyl)-2-(trifluoromethyl)-1,3-benzodioxoleHCID 178418361HCID 178418361、化合物

生成物 1

HCID 53895814HCID 53895814、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-dccbff797dcf4cf2a342bdcee39e6638
出典データセット
uspto-grants-1995_05
特許番号
US05420309

反応ノート

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