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

HRID 1081298ノート

反応式

HRID 1081298 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 from Example 17a were dissolved in 2,000 ml of tetrahydrofuran, and 20 g of catalyst (palladium on carbon, 5% by weight) were added. Hydrogenation was carried out with hydrogen at 25 to 30 bar for 13 hours at room temperature. The mixture was then filtered and the solvent 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 mixture was then filtered

出典と根拠

ORDレコード
ord-85c5a3b56c1a4e54b170baa95c149821
出典データセット
uspto-grants-1996_12
特許番号
US05585395

反応ノート

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