2,3-Dihydrofuran → HCID 66735283, 화합물

HRID 645303노트

반응식

HRID 645303 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([C:9]([C:22]([F:25])([F:24])[F:23])=[CH:10][C:11]([C:13]2[CH:21]=[CH:20][C:16]([C:17]([NH2:19])=[O:18])=[CH:15][CH:14]=2)=[O:12])[CH:5]=[C:6]([Cl:8])[CH:7]=1.[O:26]1[CH:30]=[CH:29][CH2:28][CH2:27]1.O.C1(C)C=CC(S(O)(=O)=O)=CC=1>ClCCl>[Cl:1][C:2]1[CH:3]=[C:4]([C:9]([C:22]([F:25])([F:23])[F:24])=[CH:10][C:11]([C:13]2[CH:21]=[CH:20][C:16]([C:17]([NH:19][CH:27]3[CH2:28][CH2:29][CH2:30][O:26]3)=[O:18])=[CH:15][CH:14]=2)=[O:12])[CH:5]=[C:6]([Cl:8])[CH:7]=1

참가 물질

5

반응물 3

HCID 709342,3-DihydrofuranHCID 521998p-Toluenesulfonic acid monohydrateHCID 66735592HCID 66735592, 화합물

생성물 1

HCID 66735283HCID 66735283, 화합물수율 40.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 0.25 g of 4-(3-(3,5-dichlorophenyl)-4,4,4-trifluoro-2-butenoyl)benzoic acid amide that was synthesized under Synthetic Example 9 in 3 mL of dichloromethane, 68 mg of 2,3-dihydrofuran and a catalytic amount of p-toluenesulfonic acid monohydrate were added and the mixture was stirred for 18 hours at room temperature. The solvent was distilled off from the reaction solution under reduced pressure, and the resulting residue was purified using silica gel column chromatography that was eluted with ethyl acetate-hexane (2:3) followed by crystallization from a mixed solvent of hexane and a small amount of ethyl acetate to obtain 0.12 g of aimed product as yellow solid.

후처리

  1. distillationThe solvent was distilled off from the reaction solution under reduced pressure
  2. customthe resulting residue was purified
  3. washwas eluted with ethyl acetate-hexane (2:3)
  4. customfollowed by crystallization from a mixed solvent of hexane

출처 및 근거

ORD 기록
ord-54e0e0e88d89496ea2a66552cf447732
출처 데이터셋
uspto-grants-2010_04
특허 번호
US07700808B2

반응 노트

불러오는 중…