Hydrochloric Acid → 4-[(3,5-difluorobenzyl)amino]-6-(1H-pyrrolo[2,3-b]pyridin-3-yl)pyridine-3-carboxyamide

HRID 2035544ノート

反応式

HRID 2035544 の反応式
[F:1][C:2]1[CH:3]=[C:4]([CH:36]=[C:37]([F:39])[CH:38]=1)[CH2:5][NH:6][C:7]1[CH:12]=[C:11]([C:13]2[C:21]3[C:16](=[N:17][CH:18]=[CH:19][CH:20]=3)[N:15](S(C3C=CC(C)=CC=3)(=O)=O)[CH:14]=2)[N:10]=[CH:9][C:8]=1[CH2:32][C:33]([NH2:35])=[O:34].Cl>CO.[OH-].[Na+].O>[F:39][C:37]1[CH:36]=[C:4]([CH:3]=[C:2]([F:1])[CH:38]=1)[CH2:5][NH:6][C:7]1[CH:12]=[C:11]([C:13]2[C:21]3[C:16](=[N:17][CH:18]=[CH:19][CH:20]=3)[NH:15][CH:14]=2)[N:10]=[CH:9][C:8]=1[CH2:32][C:33]([NH2:35])=[O:34]

参加物

6

反応物 2

HCID 313Hydrochloric AcidHCID 1317310074-[(3,5-difluorobenzyl)amino]-6-{1-[(4-methylphenyl)sulfonyl]-1H-pyrrolo[2,3-b]pyridin-3-yl}pyridine-3-carboxyamide2 回

生成物 1

HCID 1317310084-[(3,5-difluorobenzyl)amino]-6-(1H-pyrrolo[2,3-b]pyridin-3-yl)pyridine-3-carboxyamide収率 41%

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 962Water溶媒HCID 14798Sodium Hydroxide溶媒

実験手順

10 mg of 4-[(3,5-difluorobenzyl)amino]-6-{1-[(4-methylphenyl)sulfonyl]-1H-pyrrolo[2,3-b]pyridin-3-yl}pyridine-3-carboxyamide (the compound of Example 370) was dissolved in 0.5 mL of methanol, to which 0.5 mL of 6 mol/L sodium hydroxide in water was added, and stirred at room temperature for 4 hours. Under ice cooling, hydrochloric acid was added to acidify (about pH 1) the reaction mixture, and washed with chloroform. The aqueous layer was basified (about pH 8) with saturated sodium bicarbonate in water, extracted with chloroform, the extract was washed with water, and dried on anhydrous sodium sulfate. The solvent was evaporated to obtain 2.9 mg (yield 41%) of the title compound as a white solid.

後処理

  1. additionwas added
  2. washwashed with chloroform
  3. extractionextracted with chloroform
  4. washthe extract was washed with water
  5. dry with materialdried on anhydrous sodium sulfate
  6. customThe solvent was evaporated

出典と根拠

ORDレコード
ord-3bd447680646492cab124c2533f966d8
出典データセット
uspto-grants-2013_11
特許番号
US08575153B2

反応ノート

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