3,5-Dimethylisoxazole-4-isocyanate → HCID 10109195、化合物

HRID 396291

反応式

HRID 396291 の反応式
[NH2:1][C:2]1[C:3]([OH:13])=[C:4]([S:9]([NH2:12])(=[O:11])=[O:10])[C:5]([Cl:8])=[CH:6][CH:7]=1.[CH3:14][C:15]1[C:19]([N:20]=[C:21]=[O:22])=[C:18]([CH3:23])[O:17][N:16]=1>CN(C)C=O>[NH2:12][S:9]([C:4]1[C:3]([OH:13])=[C:2]([NH:1][C:21]([NH:20][C:19]2[C:15]([CH3:14])=[N:16][O:17][C:18]=2[CH3:23])=[O:22])[CH:7]=[CH:6][C:5]=1[Cl:8])(=[O:11])=[O:10]

参加物

4

反応物 2

HCID 27362663,5-Dimethylisoxazole-4-isocyanateHCID 113680593-Amino-6-chloro-2-hydroxy-benzenesulfonamide

生成物 1

HCID 10109195HCID 10109195、化合物収率 49%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Under Ar, a solution of 3-amino-6-chloro-2-hydroxybenzenesulfonamide (50 mg, 0.23 mmol) and 3,5-dimethylisoxazol4-yl isocyanate (31 mg, 0.23 mmol) in 1.0 mL of N,N-dimethyl-formamide was stirred at room temperature for 20 hours. Purification upon Gilson HPLC, eluting with acetonitrile/water (10/90, v/v to 90/10, v/v, over 10 min), gave the desired product (40 mg, 49%). LC-MS (m/z) 361.0 (M+).

後処理

  1. customPurification upon Gilson HPLC
  2. washeluting with acetonitrile/water (10/90, v/v to 90/10

出典と根拠

ORDレコード
ord-6457942f5bfa486ab44bb958b4e1db83
出典データセット
uspto-grants-2003_08
特許番号
US06608077B2

関連ノート

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