Dimethylamine → 2-(2'-Methoxy-4'-dimethylaminosulfonyl-phenyl)-imidazo[4,5-b]pyridine hydrochloride

HRID 2309884

反応式

HRID 2309884 の反応式
Cl.[CH3:2][O:3][C:4]1[CH:9]=[C:8]([S:10]([Cl:13])(=[O:12])=[O:11])[CH:7]=[CH:6][C:5]=1[C:14]1[NH:15][C:16]2[C:17]([N:22]=1)=[N:18][CH:19]=[CH:20][CH:21]=2.COC1C=C(S(Cl)(=O)=O)C=CC=1C(O)=O.[CH3:38][NH:39][CH3:40]>>[ClH:13].[CH3:2][O:3][C:4]1[CH:9]=[C:8]([S:10]([N:39]([CH3:40])[CH3:38])(=[O:12])=[O:11])[CH:7]=[CH:6][C:5]=1[C:14]1[NH:15][C:16]2[C:17]([N:22]=1)=[N:18][CH:19]=[CH:20][CH:21]=2

参加物

4

反応物 3

HCID 674DimethylamineHCID 201845172-(2'-Methoxy-4'-chlorosulfonyl-phenyl)-imidazo[4,5-b]pyridine hydrochlorideHCID 201845804-(Chlorosulfonyl)-2-methoxybenzoic acid

生成物 1

HCID 201845662-(2'-Methoxy-4'-dimethylaminosulfonyl-phenyl)-imidazo[4,5-b]pyridine hydrochloride

実験手順

The crude 2-(2'-methoxy-4'-chlorosulfonyl-phenyl)-imidazo[4,5-b]pyridine hydrochloride prepared from 2.5 gm of 2-methoxy-4-chlorosulfonyl-benzoic acid according to Example C was added to 150 ml of a saturated aqueous dimethylamine solution at 10° C., under stirring, and a light-colored precipitate formed slowly. After stirring for 20 hours at ambient temperature, 200 ml of ice water were added. The precipitate was dried and then taken up in 60 ml of methanol, and 10 ml of methanolic hydrochloric acid were added. After filtering over active charcoal, the solvent was eliminated, and the residue remaining was digested with acetone and ether, subjected to suction filtration, and washed with ether.

後処理

  1. customa light-colored precipitate formed slowly
  2. stirringAfter stirring for 20 hours at ambient temperature
  3. customThe precipitate was dried
  4. addition10 ml of methanolic hydrochloric acid were added
  5. filtrationAfter filtering over active charcoal
  6. filtrationsubjected to suction filtration
  7. washwashed with ether

出典と根拠

ORDレコード
ord-b0531ecf3c564a98af57cd6405a0dd48
出典データセット
uspto-grants-1987_09
特許番号
US04696931

関連ノート

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