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Sodium Bicarbonate → HCID 178527470、化合物

HRID 1173107
ノート
印刷プレビュー

反応式

HRID 1173107 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

HCID 178527470HCID 178527470、化合物収率 53.8%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-94c66f15fcc54269b47692b7bfbac555
出典データセット
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07834049B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート