Acetic Acid → HCID 13345321, 화합물

HRID 1011333노트

반응식

HRID 1011333 반응식
[CH3:1][C:2]1[N:7](C(O)=O)[CH:6]([C:11]([OH:13])=[O:12])[CH:5]=[CH:4][CH:3]=1.[C:14](O)(=[O:16])C.N1C=CC=CC=1.CCCCCC>COCCOC.CCOCC>[CH3:1][C:2]1[N:7]=[C:6]2[C:11](=[O:12])[O:13][C:14](=[O:16])[C:5]2=[CH:4][CH:3]=1

참가 물질

7

반응물 4

HCID 176Acetic AcidHCID 1049PyridineHCID 8058HexaneHCID 67315455HCID 67315455, 화합물

생성물 1

HCID 13345321HCID 13345321, 화합물수율 74.2%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 80711,2-Dimethoxyethane용매

실험 절차

A solution of 6-methyl-1,2-pyridine dicarboxylic acid (25 g, 138 mmol) and acetic acid (42 mL, 733 mmol) in DME (150 mL) is treated with pyridine (22 mL, 272 mmol) and stirred at room temperature for 2 h. The pale yellow solution is diluted with ether (250 mL) and then hexane (1250 mL) is added slowly. A white precipitate is formed. The solution is cooled to 0° C. for 30 min and the white solid is collected by filtration. The solid is washed with hexane and dried to give the title compound as a white solid (16.7 g, 74%).

후처리

  1. customA white precipitate is formed
  2. temperatureThe solution is cooled to 0° C. for 30 min
  3. filtrationthe white solid is collected by filtration
  4. washThe solid is washed with hexane
  5. customdried

출처 및 근거

ORD 기록
ord-0696e96a5a6847609df9f444b7c2846a
출처 데이터셋
uspto-grants-2011_07
특허 번호
US07977351B2

반응 노트

불러오는 중…