Hydrochloric Acid → 2-Chloro-N-[3-chloro-4-(trifluoromethyl)benzyl]-4-[(1,2,4-thiadiazol-5-ylamino)sulfonyl]benzamide

HRID 401741

反応式

HRID 401741 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([S:23](Cl)(=[O:25])=[O:24])[CH:5]=[CH:6][C:7]=1[C:8]([NH:10][CH2:11][C:12]1[CH:17]=[CH:16][C:15]([C:18]([F:21])([F:20])[F:19])=[C:14]([Cl:22])[CH:13]=1)=[O:9].[NH2:27][C:28]1[S:32][N:31]=[CH:30][N:29]=1.Cl>>[Cl:1][C:2]1[CH:3]=[C:4]([S:23]([NH:27][C:28]2[S:32][N:31]=[CH:30][N:29]=2)(=[O:25])=[O:24])[CH:5]=[CH:6][C:7]=1[C:8]([NH:10][CH2:11][C:12]1[CH:17]=[CH:16][C:15]([C:18]([F:21])([F:20])[F:19])=[C:14]([Cl:22])[CH:13]=1)=[O:9]

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 2902745-Amino-1,2,4-thiadiazoleHCID 577321163-Chloro-4-({[3-chloro-4-(trifluoromethyl)benzyl]amino}carbonyl)benzenesulfonyl chloride

生成物 1

HCID 577321642-Chloro-N-[3-chloro-4-(trifluoromethyl)benzyl]-4-[(1,2,4-thiadiazol-5-ylamino)sulfonyl]benzamide

実験手順

The title compound was prepared from 3-chloro-4-({[3-chloro-4-(trifluoromethyl)benzyl]amino}carbonyl)benzenesulfonyl chloride (Preparation 38) and 5-amino-1,2,4-thiadiazole in following Method H described for Example 6. The reaction mixture was added to 2M HCl, extracted into ethyl acetate, dried over sodium sulphate, filtered and evaporated. The crude material was purified by column chromatography eluting with DCM:MeOH:AcOH (95:5:0.5) to yield the title compound.

後処理

  1. extractionextracted into ethyl acetate
  2. dry with materialdried over sodium sulphate
  3. filtrationfiltered
  4. customevaporated
  5. customThe crude material was purified by column chromatography
  6. washeluting with DCM:MeOH:AcOH (95:5:0.5)

出典と根拠

ORDレコード
ord-0e6a0d02d97841139f790bc6ce965d1a
出典データセット
uspto-grants-2014_06
特許番号
US08741934B2

関連ノート

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