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Sodium Bicarbonate → HCID 178527470, 화합물

HRID 1173107
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HRID 1173107 반응식
N[C:2]1[N:7]=[CH:6][C:5]([S:8]([NH:11][C:12]2[CH:13]=[CH:14][CH:15]=[C:16]3[C:20]=2[NH:19][CH:18]=[C:17]3[Cl:21])(=[O:10])=[O:9])=[CH:4][CH:3]=1.N([O-])=[O:23].[Na+].C(=O)(O)[O-].[Na+]>C(O)(=O)C>[Cl:21][C:17]1[C:16]2[C:20](=[C:12]([NH:11][S:8]([C:5]3[CH:6]=[N:7][C:2]([OH:23])=[CH:3][CH:4]=3)(=[O:10])=[O:9])[CH:13]=[CH:14][CH:15]=2)[NH:19][CH:18]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 516892Sodium BicarbonateHCID 98186186-amino-N-(3-chloro-1H-indol-7-yl)pyridine-3-sulfonamideHCID 23668193Sodium Nitrite

생성물 1

HCID 178527470HCID 178527470, 화합물수율 53.8%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

Under ice-cooling, into a solution of the compound of Example 33a (100 mg, 0.31 mmol) dissolved in 2 ml of glacial acetic acid was added dropwise 1 ml of an aqueous solution containing 32 mg (0.46 mmol) of sodium nitrite. After stirring for one hour, the mixture was adjusted to about pH 8 by adding an aqueous sodium bicarbonate and further stirred for 10 minutes. The reaction mixture was extracted with ethyl acetate, and the extract was washed with water, dried over magnesium sulfate and concentrated. Then, the residue was purified by silica gel thin layer chromatography, to give 54 mg of the title compound.

후처리

  1. stirringfurther stirred for 10 minutes
  2. extractionThe reaction mixture was extracted with ethyl acetate
  3. washthe extract was washed with water
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated
  6. customThen, the residue was purified by silica gel thin layer chromatography

출처 및 근거

ORD 기록
ord-94c66f15fcc54269b47692b7bfbac555
출처 데이터셋
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07834049B2

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