Potassium Carbonate → HCID 21192582、化合物

HRID 1068048ノート

反応式

HRID 1068048 の反応式
[Cl:1][C:2]1[CH:23]=[CH:22][C:5]([CH2:6][NH:7][C:8]([C:10]2[CH:11]=[N:12][C:13]3[C:18]([C:19]=2[OH:20])=[CH:17][C:16]([I:21])=[CH:15][CH:14]=3)=[O:9])=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].C1(C)C=C(C)C=C(C)C=1S(O[NH2:42])(=O)=O>CN(C=O)C>[NH2:42][N:12]1[C:13]2[C:18](=[CH:17][C:16]([I:21])=[CH:15][CH:14]=2)[C:19](=[O:20])[C:10]([C:8]([NH:7][CH2:6][C:5]2[CH:4]=[CH:3][C:2]([Cl:1])=[CH:23][CH:22]=2)=[O:9])=[CH:11]1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 11830845O-(2,4,6-Trimethylbenzenesulfonyl)hydroxylamineHCID 178522879HCID 178522879、化合物

生成物 1

HCID 21192582HCID 21192582、化合物収率 65.3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A suspension of N-(4-chlorobenzyl)-4-hydroxy-6-iodo-3-quinolinecarboxamide (2.0 g) of Preparation No. 4 and of potassium carbonate (2.0 g) in DMF (40 mL) is stirred at room temperature for 5 hrs and then treated with of O-(mesitylsulfonyl)hydroxylamine (1.5 g). After 24 hrs, the solvent is evaporated under reduced pressure and the residue is diluted with water(150 mL). The resulting solid is filtered and washed with water (3×) and ether (2×). Recrystallization from hot acetic acid/water affords 1.35 g of the title compound as a tan solid.

後処理

  1. customthe solvent is evaporated under reduced pressure
  2. additionthe residue is diluted with water(150 mL)
  3. filtrationThe resulting solid is filtered
  4. washwashed with water (3×) and ether (2×)
  5. customRecrystallization from hot acetic acid/water

出典と根拠

ORDレコード
ord-9c052d243c2448f1af0576a63a32754b
出典データセット
uspto-grants-2001_06
特許番号
US06248739B1

反応ノート

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