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Sodium Hydroxide → 2-(4-Fluorophenyl)-4-methylpyrimidine-5-carboxylic acid

HRID 219656
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인쇄 미리보기

반응식

HRID 219656 반응식
C([O:3][C:4]([C:6]1[C:7]([CH3:19])=[N:8][C:9]([C:12]2[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=2)=[N:10][CH:11]=1)=[O:5])C.[OH-].[Na+]>CO>[F:18][C:15]1[CH:14]=[CH:13][C:12]([C:9]2[N:8]=[C:7]([CH3:19])[C:6]([C:4]([OH:5])=[O:3])=[CH:11][N:10]=2)=[CH:17][CH:16]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 69279303Ethyl-2-(4-fluorophenyl)-4-methylpyrimidine-5-carboxylate

생성물 1

HCID 300316142-(4-Fluorophenyl)-4-methylpyrimidine-5-carboxylic acid수율 88.2%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of ethyl-2-(4-fluorophenyl)-4-methylpyrimidine-5-carboxylate (1.65 g, 6.35 mmol) in MeOH (75 mL) is treated with 2 N aqueous sodium hydroxide (10 mL) and heated to reflux for 30 min. MeOH is removed in vacuo and the residue is diluted with water (50 mL). The solution is adjusted to pH ˜2 with 2 M hydrochloric acid. The precipitated is collected by filtration, washed with water and vacuum dried to afford 2-(4-fluorophenyl)-4-methylpyrimidine-5-carboxylic acid (1.3 g, 88%) as a solid. MS: 233 (M+H).

후처리

  1. temperatureheated
  2. temperatureto reflux for 30 min
  3. customMeOH is removed in vacuo
  4. additionthe residue is diluted with water (50 mL)
  5. filtrationThe precipitated is collected by filtration
  6. washwashed with water and vacuum
  7. customdried

출처 및 근거

ORD 기록
ord-7b8000808ed0476f9b375b0775826a57
출처 데이터셋
uspto-grants-2012_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08202863B2

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