Chloroacetic Acid → (2-Imino-2H-pyridin-1-yl)-acetic acid

HRID 1804694노트

반응식

HRID 1804694 반응식
Cl[CH2:2][C:3]([OH:5])=[O:4].C(N(CC)CC)C.[NH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][N:15]=1>O.C(O)C>[NH:13]=[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][N:15]1[CH2:2][C:3]([OH:5])=[O:4]

참가 물질

6

반응물 3

HCID 300Chloroacetic AcidHCID 8471TriethylamineHCID 104392-Aminopyridine

생성물 1

HCID 10997222(2-Imino-2H-pyridin-1-yl)-acetic acid

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

반응 조건

온도
90 °C

실험 절차

In a 100 mL round bottom flask, 2-chloroacetic acid (10 g, 106 mmol) in water (16.3 mL) was treated with triethylamine (16.67 mL, 120 mmol) dropwise over 6 minutes. After stirring the reaction at ambient temperature for 10 minutes, 2-aminopyridine (11.76 g, 125 mmol) was added and the mixture was heated at 90° C. for 5 hours. The reaction mixture was cooled to ambient temperature and diluted with ethanol (11 mL). The resulting suspension was stirred in an ice bath for 1 hour and filtered. The solid collected was washed with ˜30 mL cold ethanol and dried under vacuum to constant weight to provide the title compound. MS (DCI(+)) m/e 152.9 (M+H)+.

후처리

  1. customthe reaction at ambient temperature for 10 minutes
  2. temperatureThe reaction mixture was cooled to ambient temperature
  3. stirringThe resulting suspension was stirred in an ice bath for 1 hour
  4. filtrationfiltered
  5. customThe solid collected
  6. washwas washed with ˜30 mL cold ethanol
  7. customdried under vacuum to constant weight

출처 및 근거

ORD 기록
ord-d6ac98d55b734229b0349b49bfb0a888
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08354422B2

반응 노트

불러오는 중…