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

HRID 1081298노트

반응식

HRID 1081298 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 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.

후처리

  1. filtrationThe mixture was then filtered

출처 및 근거

ORD 기록
ord-85c5a3b56c1a4e54b170baa95c149821
출처 데이터셋
uspto-grants-1996_12
특허 번호
US05585395

반응 노트

불러오는 중…