Hydrochloric Acid → HCID 9892985, 화합물

HRID 1066508

반응식

HRID 1066508 반응식
[CH3:1][O:2][C:3]1[C:8]([O:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[O:16][CH3:17])=[C:7]([NH:18][S:19]([C:22]2[CH:27]=[CH:26][C:25]([CH3:28])=[CH:24][N:23]=2)(=[O:21])=[O:20])[N:6]=[C:5]([C:29]2[CH:34]=[CH:33][N:32]=[C:31]([C:35](N)=[O:36])[CH:30]=2)[N:4]=1.Cl.C1C[O:42]CC1>C1COCC1.O1CCOCC1>[CH3:1][O:2][C:3]1[C:8]([O:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[O:16][CH3:17])=[C:7]([NH:18][S:19]([C:22]2[CH:27]=[CH:26][C:25]([CH3:28])=[CH:24][N:23]=2)(=[O:21])=[O:20])[N:6]=[C:5]([C:29]2[CH:34]=[CH:33][N:32]=[C:31]([C:35]([OH:42])=[O:36])[CH:30]=2)[N:4]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric Acid2회HCID 8028TetrahydrofuranHCID 537796624-[4-Methoxy-5-(2-methoxy-phenoxy)-6-(5-methyl-pyridine-2-sulfonylamino)-pyrimidin-2-yl]-pyridine-2-carboxylic acid amide2회

생성물 1

HCID 9892985HCID 9892985, 화합물

시약·촉매·용매 1

HCID 22018518Dioxane tetrahydrofuran용매

실험 절차

1 g of 4-[4-methoxy-5-(2-methoxy-phenoxy)-6-(5-methyl-pyridine-2-sulfonylamino)-pyrimidin-2-yl]-pyridine-2-carboxylic acid amide, product of example 20, dissolved in a mixture of THF/dioxane (40 ml/30 ml) were treated at RT with 3N HCl (40 ml) and the solution was refluxed for 24 h, further THF (12 ml) and 3M HCl (12 ml) was then added and the solution was heated to reflux for further 24 h until the transformation was complete according to TLC analysis. The reaction mixture was concentrated in vacuo and the product was extracted into CH2Cl2. The organic layer was dried over Na2SO4, the solvent removed in vacuo. The remaining crystalline solid was washed with ether and dried in a vacuum to give 4-[4-methoxy-5-(2-methoxy-phenoxy)-6-(5-methyl-pyridine-2-sulfonylamino)-pyrimidin-2-yl]-pyridine-2-carboxylic acid as an off-white solid. ISN mass spectrum, m/e 522 (M−1 calculated for C24H21N5O7S: 522).

후처리

  1. temperaturethe solution was refluxed for 24 h
  2. temperaturethe solution was heated
  3. temperatureto reflux for further 24 h until the transformation
  4. concentrationThe reaction mixture was concentrated in vacuo
  5. extractionthe product was extracted into CH2Cl2
  6. dry with materialThe organic layer was dried over Na2SO4
  7. customthe solvent removed in vacuo
  8. washThe remaining crystalline solid was washed with ether
  9. customdried in a vacuum

출처 및 근거

ORD 기록
ord-600c67ba4942435185fd967c366acc41
출처 데이터셋
uspto-grants-2001_06
특허 번호
US06242601B1

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