Hydrochloric Acid → N-(4-biphenyl-3-yl-thiazol-2-yl)-4-methyl-benzenesulfonamide

HRID 1417284ノート

反応式

HRID 1417284 の反応式
[C:1]1([C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[CH:6]=[CH:5][CH:4]=[C:3]([C:7]2[N:8]=[C:9]([N:12](COC)[S:13]([C:16]3[CH:21]=[CH:20][C:19]([CH3:22])=[CH:18][CH:17]=3)(=[O:15])=[O:14])[S:10][CH:11]=2)[CH:2]=1.Cl.O>O1CCCC1>[C:1]1([C:26]2[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=2)[CH:6]=[CH:5][CH:4]=[C:3]([C:7]2[N:8]=[C:9]([NH:12][S:13]([C:16]3[CH:21]=[CH:20][C:19]([CH3:22])=[CH:18][CH:17]=3)(=[O:15])=[O:14])[S:10][CH:11]=2)[CH:2]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 962WaterHCID 21845572N-(4-biphenyl-3-yl-thiazol-2-yl)-N-methoxymethyl-4-methyl-benzenesulfonamide

生成物 1

HCID 21845585N-(4-biphenyl-3-yl-thiazol-2-yl)-4-methyl-benzenesulfonamide収率 45.9%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of 0.29 g of N-(4-biphenyl-3-yl-thiazol-2-yl)-N-methoxymethyl-4-methyl-benzenesulfonamide in 6 ml of tetra-hydrofuran was stirred at room temperature for 6 hours after the addition of 1.5 ml of 6N hydrochloric acid. The reaction mixture was added to 40 ml of water and extracted with ethyl acetate. The organic phases were combined, dried with magnesium sulphate and concentrated. Recrystallization from 10 ml of 50% ethanol yielded 120 mg of N-(4-biphenyl-3-yl-thiazol-2-yl)-4-methyl-benzenesulfonamide as colorless crystals.

後処理

  1. extractionextracted with ethyl acetate
  2. dry with materialdried with magnesium sulphate
  3. concentrationconcentrated
  4. customRecrystallization from 10 ml of 50% ethanol

出典と根拠

ORDレコード
ord-485f8b76b32441aead511284301b7f8c
出典データセット
uspto-grants-1999_03
特許番号
US05877193

反応ノート

読み込み中…