Sodium Hydroxide → HCID 58835252、化合物

HRID 1660912ノート

反応式

HRID 1660912 の反応式
C[O:2][C:3](=[O:35])[C:4]1[C:9]([NH:10][C:11]2[C:12]3[CH:28]=[CH:27][C:26]([NH:29][CH2:30][CH2:31][N:32]([CH3:34])[CH3:33])=[N:25][C:13]=3[N:14]=[C:15]([C:17]3[CH:22]=[C:21]([Cl:23])[CH:20]=[CH:19][C:18]=3[F:24])[N:16]=2)=[CH:8][CH:7]=[N:6][CH:5]=1.[OH-].[Na+]>CO>[Cl:23][C:21]1[CH:20]=[CH:19][C:18]([F:24])=[C:17]([C:15]2[N:16]=[C:11]([NH:10][C:9]3[C:4]([C:3]([OH:35])=[O:2])=[CH:5][N:6]=[CH:7][CH:8]=3)[C:12]3[CH:28]=[CH:27][C:26]([NH:29][CH2:30][CH2:31][N:32]([CH3:34])[CH3:33])=[N:25][C:13]=3[N:14]=2)[CH:22]=1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 58835245HCID 58835245、化合物

生成物 1

HCID 58835252HCID 58835252、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a suspension of the ester, 4-[2-(5-Chloro-2-fluoro-phenyl)-7-(2-dimethylamino-ethylamino)-pyrido[2,3-d]pyrimidin-4-ylamino]-nicotinic acid methyl ester (0.300 g) in MeOH (20 ml) was added a 1N NaOH (aq) (1.0 ml) and the reaction mixture was heated to reflux for 2 h. The solution was cooled to rt and concentrated in vacuo. Water (50 ml) was added to the crude material and the aqueous layer was acidified with HCl (1 N) and the mixture was placed in the freezer. The solid was filtered, washed with water and dried to give 4-[2-(5-Chloro-2-fluorophenyl)-7-(2-dimethylamino-ethylamino)-pyrido[2,3-d]pyrimidin-4-ylamino]-nicotinic acid as a cream colored solid. This material was used without further purification.

後処理

  1. temperaturethe reaction mixture was heated
  2. temperatureto reflux for 2 h
  3. concentrationconcentrated in vacuo
  4. additionWater (50 ml) was added to the crude material
  5. filtrationThe solid was filtered
  6. washwashed with water
  7. customdried

出典と根拠

ORDレコード
ord-646e877f299b419ba1b4b111294c29b5
出典データセット
uspto-grants-2011_10
特許番号
US08030318B2

反応ノート

読み込み中…