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

HRID 343836노트

반응식

HRID 343836 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

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.

후처리

  1. filtrationThe batch was then filtered

출처 및 근거

ORD 기록
ord-47c2d22b9bbe47d2879d0df24c1ade88
출처 데이터셋
uspto-grants-1999_01
특허 번호
US05863933

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