Sodium Hydroxide → HCID 58835252, 화합물

HRID 1660912노트

반응식

HRID 1660912 반응식
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

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 58835245HCID 58835245, 화합물

생성물 1

HCID 58835252HCID 58835252, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-646e877f299b419ba1b4b111294c29b5
출처 데이터셋
uspto-grants-2011_10
특허 번호
US08030318B2

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