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Potassium Carbonate → HCID 23666225, 화합물

HRID 486610
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HRID 486610 반응식
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]2[C:14]([NH:15][S:16]([C:19]3[CH:24]=[CH:23][C:22]([O:25][CH3:26])=[CH:21][CH:20]=3)(=[O:18])=[O:17])=[CH:13][CH:12]=[CH:11][N:10]=2)=[CH:4][CH:3]=1.Cl[S:28]([OH:31])(=[O:30])=[O:29].C(=O)([O-])[O-].[K+:36].[K+]>N1C=CC=CC=1>[S:28]([O-:31])([O:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]2[C:14]([NH:15][S:16]([C:19]3[CH:24]=[CH:23][C:22]([O:25][CH3:26])=[CH:21][CH:20]=3)(=[O:18])=[O:17])=[CH:13][CH:12]=[CH:11][N:10]=2)=[CH:4][CH:3]=1)(=[O:30])=[O:29].[K+:36]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 24638Chlorosulfonic acidHCID 3035714N-[2-[(4-Hydroxyphenyl)amino]-3-pyridinyl]-4-methoxybenzenesulfonamide

생성물 1

HCID 23666225HCID 23666225, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

2.0 g (5.38 mmol) of the compound of Example 6 was dissolved in 20 ml of pyridine. 800 mg (6.87 mmol) of chlorosulfonic acid (95%) was added dropwise thereto at -15° to -10° C. The temperature was slowly elevated to room temperature and the mixture was stirred for 3 days. A 1N aqueous potassium carbonate solution was added to the reaction mixture to adjust the pH to 8 to 9. The solvent was distilled off under reduced pressure. Water and ethyl acetate were added to the residue and an aqueous layer thus formed was separated, concentrated, purified by silica gel column chromatography and precipitated with methanol/dichloromethane to obtain 1.58 g of the title compound.

후처리

  1. customat -15° to -10° C
  2. customwas slowly elevated to room temperature
  3. distillationThe solvent was distilled off under reduced pressure
  4. additionWater and ethyl acetate were added to the residue
  5. customan aqueous layer thus formed
  6. customwas separated
  7. concentrationconcentrated
  8. custompurified by silica gel column chromatography
  9. customprecipitated with methanol/dichloromethane

출처 및 근거

ORD 기록
ord-07c664627c514fcd9ea2dcaf1bfd2c45
출처 데이터셋
uspto-grants-1994_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05292758

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