Potassium Carbonate → HCID 21192582, 화합물

HRID 1068048노트

반응식

HRID 1068048 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 21192582HCID 21192582, 화합물수율 65.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9c052d243c2448f1af0576a63a32754b
출처 데이터셋
uspto-grants-2001_06
특허 번호
US06248739B1

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