Carbon Tetrachloride → HCID 18954841, 화합물

HRID 2380662노트

반응식

HRID 2380662 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:12]([C:13]3[CH:18]=[CH:17][C:16]([F:19])=[CH:15][CH:14]=3)=[CH:11][C:10]([C:20]([NH:22][C:23]3[CH:28]=[CH:27][C:26]([C:29]([F:32])([F:31])[F:30])=[CH:25][CH:24]=3)=O)=[N:9]2)=[CH:4][CH:3]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(Cl)(Cl)(Cl)[Cl:53]>C(#N)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH:12]([C:13]3[CH:18]=[CH:17][C:16]([F:19])=[CH:15][CH:14]=3)[CH2:11][C:10]([C:20]([Cl:53])=[N:22][C:23]3[CH:28]=[CH:27][C:26]([C:29]([F:32])([F:31])[F:30])=[CH:25][CH:24]=3)=[N:9]2)=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 5943Carbon TetrachlorideHCID 11776TriphenylphosphineHCID 18954839HCID 18954839, 화합물

생성물 1

HCID 18954841HCID 18954841, 화합물수율 154.2%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To a solution of 2.50 g (0.0054 mol) of 1-(4-chlorophenyl)-5-(4-fluorophenyl)-N-[4-(trifluoromethyl)-phenyl]-1H-pyrazole-3-carboxamide dissolved in 15 mL of acetonitrile was added 1.80 g (0.0067 mol) of triphenylphosphine and 0.83 g (0.0054 mol) of carbon tetrachloride. The yellow solution was stirred at room temperature overnight and concentrated to afford 4.0 g of a yellow solid. The crude product was chromatographed on silica gel using ethyl acetate (10%) and hexanes (90%) as eluents which afforded 0.64 g of a yellow solid, mp 154° C. to 156° C.

후처리

  1. concentrationconcentrated

출처 및 근거

ORD 기록
ord-e5b0dade0bfe440b82d6cf72c4fd4edc
출처 데이터셋
uspto-grants-1994_11
특허 번호
US05369121

반응 노트

불러오는 중…