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

HRID 343836ノート

反応式

HRID 343836 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

339 g of the product of Example 17a were dissolved in 2000 ml of tetrahydrofuran and treated with 20 g of catalyst (palladium on charcoal, 5% strength by weight). The mixture was hydrogenated with hydrogen for 13 hours at 25 to 30 bar and at room temperature. The batch was then filtered and the solvent was stripped off in vacuo. A solid remained. 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. filtrationThe batch was then filtered

出典と根拠

ORDレコード
ord-47c2d22b9bbe47d2879d0df24c1ade88
出典データセット
uspto-grants-1999_01
特許番号
US05863933

反応ノート

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