Sodium Hydroxide → 1-[2-(2-Chloro-benzylamino)-pyrido[4,3-d]pyrimidin-5-yl]-piperidine-4-carboxylic acid

HRID 41484노트

반응식

HRID 41484 반응식
C([O:3][C:4]([CH:6]1[CH2:11][CH2:10][N:9]([C:12]2[C:21]3[CH:20]=[N:19][C:18]([NH:22][CH2:23][C:24]4[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=4[Cl:30])=[N:17][C:16]=3[CH:15]=[CH:14][N:13]=2)[CH2:8][CH2:7]1)=[O:5])C.[OH-].[Na+]>C1COCC1>[Cl:30][C:25]1[CH:26]=[CH:27][CH:28]=[CH:29][C:24]=1[CH2:23][NH:22][C:18]1[N:19]=[CH:20][C:21]2[C:12]([N:9]3[CH2:8][CH2:7][CH:6]([C:4]([OH:5])=[O:3])[CH2:11][CH2:10]3)=[N:13][CH:14]=[CH:15][C:16]=2[N:17]=1

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 584501201-[2-(2-Chloro-benzylamino)-pyrido[4,3-d]pyrimidin-5-yl]-piperidine-4-carboxylic acid ethyl ester

생성물 1

HCID 208551921-[2-(2-Chloro-benzylamino)-pyrido[4,3-d]pyrimidin-5-yl]-piperidine-4-carboxylic acid

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
50 °C

실험 절차

1-[2-(2-Chloro-benzylamino)-pyrido[4,3-d]pyrimidin-5-yl]-piperidine-4-carboxylic acid ethyl ester 13 (583 mg, 1.37 mmol) was dissolved in THF (10 mL), 2 N NaOH solution (5 mL) were added and the mixture was stirred for 3 h at 50° C. The mixture was evaporated to dryness, water was added and the pH was adjusted to 7 adding 2 N HCl solution. The aqueous layer was extracted twice with ethyl acetate and DCM. The combined organic layers were dried over sodium sulfate, filtered and evaporated to dryness. The obtained colorless solid (447 mg, 1.12 mmol, 82%) was used without further purification.

후처리

  1. customThe mixture was evaporated to dryness, water
  2. additionwas added
  3. extractionThe aqueous layer was extracted twice with ethyl acetate and DCM
  4. dry with materialThe combined organic layers were dried over sodium sulfate
  5. filtrationfiltered
  6. customevaporated to dryness

출처 및 근거

ORD 기록
ord-2f9120211bca48e0bdf05f4ce8ff6590
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08530650B2

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