2,3-Dihydrofuran → HCID 66735283、化合物

HRID 645303ノート

反応式

HRID 645303 の反応式
[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

参加物

5

反応物 3

HCID 709342,3-DihydrofuranHCID 521998p-Toluenesulfonic acid monohydrateHCID 66735592HCID 66735592、化合物

生成物 1

HCID 66735283HCID 66735283、化合物収率 40.7%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-54e0e0e88d89496ea2a66552cf447732
出典データセット
uspto-grants-2010_04
特許番号
US07700808B2

反応ノート

読み込み中…