HCID 13292769, 화합물 → 77599-89-4

HRID 1382627노트

반응식

HRID 1382627 반응식
[N:1]([CH2:4][CH2:5][O:6][C:7]1[CH:12]=[CH:11][C:10](/[C:13](/[C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)=[C:14](\[C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)/[C:15]([F:18])([F:17])[F:16])=[CH:9][CH:8]=1)=[N+]=[N-]>CO.[Pd]>[NH2:1][CH2:4][CH2:5][O:6][C:7]1[CH:8]=[CH:9][C:10](/[C:13](/[C:25]2[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=2)=[C:14](\[C:19]2[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=2)/[C:15]([F:16])([F:17])[F:18])=[CH:11][CH:12]=1

참가 물질

4

반응물 1

HCID 13292769HCID 13292769, 화합물

생성물 1

HCID 1329277277599-89-4수율 52.6%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

7.40 g (18 mmoles) of (E)-1-[4-(2-azidoethoxy)-phenyl]-1,2-diphenyl-3,3,3-trifluoro-propene, prepared as described in Example 7, are dissolved in 100 ml of methanol, 0.70 g of a 5% palladium-on-carbon catalyst are added, and the mixture is hydrogenated for about one hour. The catalyst is filtered off, the solution is evaporated, and the residue is crystallized from hexane. 3.63 g (52.3%) of the aimed compound are obtained; m.p.: 71°-76° C.

후처리

  1. filtrationThe catalyst is filtered off
  2. customthe solution is evaporated
  3. customthe residue is crystallized from hexane

출처 및 근거

ORD 기록
ord-8acc8028724e4ab0a4db05f017fc0e64
출처 데이터셋
uspto-grants-1989_02
특허 번호
US04806685

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