Potassium Carbonate → 2,2,2-Trifluoro-N-(4-(2-methoxyphenoxy)phenyl)-N-(3-pyridinylmethyl)ethanesulfonamide

HRID 392401ノート

反応式

HRID 392401 の反応式
[CH3:1][O:2][C:3]1[CH:23]=[CH:22][CH:21]=[CH:20][C:4]=1[O:5][C:6]1[CH:11]=[CH:10][C:9]([NH:12][CH2:13][C:14]2[CH:15]=[N:16][CH:17]=[CH:18][CH:19]=2)=[CH:8][CH:7]=1.[F:24][C:25]([F:32])([F:31])[CH2:26][S:27](Cl)(=[O:29])=[O:28].C(=O)([O-])[O-].[K+].[K+]>ClCCCl.N1C=CC=CC=1>[CH3:1][O:2][C:3]1[CH:23]=[CH:22][CH:21]=[CH:20][C:4]=1[O:5][C:6]1[CH:7]=[CH:8][C:9]([N:12]([CH2:13][C:14]2[CH:15]=[N:16][CH:17]=[CH:18][CH:19]=2)[S:27]([CH2:26][C:25]([F:32])([F:31])[F:24])(=[O:29])=[O:28])=[CH:10][CH:11]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 742422,2,2-Trifluoroethanesulfonyl chlorideHCID 109904214-(2-methoxyphenoxy)-N-(pyridin-3-ylmethyl)aniline

生成物 1

HCID 98250842,2,2-Trifluoro-N-(4-(2-methoxyphenoxy)phenyl)-N-(3-pyridinylmethyl)ethanesulfonamide

試薬・触媒・溶媒 1

HCID 21470604DCE Pyridine溶媒

実験手順

A solution of N-(4-(2-methoxyphenoxy)phenyl)pyridin-3-ylmethylamine (1.0 equiv.) in 2:1 DCE/Pyridine (0.15 M) was cooled to 0° C. and treated with 2,2,2-trifluoroethanesulfonyl chloride (1.8 equiv.). The mixture was allowed to warm to ambient temperature and stir overnight. The reaction was treated with anhydrous potassium carbonate, stirred for 40 min, and filtered. The filtrate was purified via preparative HPLC eluting with 98:2 to 96:4 DCM/MeOH to give the title compound. Anal Calcd for C21H19F3N2O4S: C, 55.75; H, 4.23; N, 6.19. Found: C, 55.65; H, 4.27; N, 6.19. MS found 4.53.0 [M+H]+

後処理

  1. stirringstirred for 40 min
  2. filtrationfiltered
  3. customThe filtrate was purified via preparative HPLC
  4. washeluting with 98:2 to 96:4 DCM/MeOH

出典と根拠

ORDレコード
ord-30f3993c84af4b15b988a21505d8ce6c
出典データセット
uspto-grants-2004_10
特許番号
US06800651B2

反応ノート

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