3-(2-Fluoro-4-iodo-phenylamino)-1-methyl-1H-pyrrolo[3,2-c]pyridine-2-carboxylic acid ethyl ester → HCID 59596445, 화합물

HRID 2264900노트

반응식

HRID 2264900 반응식
C([O:3][C:4]([C:6]1[N:14]([CH3:15])[C:13]2[CH:12]=[CH:11][N:10]=[CH:9][C:8]=2[C:7]=1[NH:16][C:17]1[CH:22]=[CH:21][C:20]([I:23])=[CH:19][C:18]=1[F:24])=[O:5])C>[OH-].[Na+]>[F:24][C:18]1[CH:19]=[C:20]([I:23])[CH:21]=[CH:22][C:17]=1[NH:16][C:7]1[C:8]2[CH:9]=[N:10][CH:11]=[CH:12][C:13]=2[N:14]([CH3:15])[C:6]=1[C:4]([OH:5])=[O:3]

참가 물질

3

반응물 1

HCID 595965873-(2-Fluoro-4-iodo-phenylamino)-1-methyl-1H-pyrrolo[3,2-c]pyridine-2-carboxylic acid ethyl ester

생성물 1

HCID 59596445HCID 59596445, 화합물수율 97.3%

시약·촉매·용매 1

HCID 14798Sodium Hydroxide용매

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온도
65 °C

실험 절차

A mixture of 3-(2-fluoro-4-iodo-phenylamino)-1-methyl-1H-pyrrolo[3,2-c]pyridine-2-carboxylic acid ethyl ester (88 mg, 0.20 mmol), 1M aqueous sodium hydroxide solution (220 μl) and IMS (3 ml) was heated at 65° C. for 2 hours. After cooling to ambient temperature the solvent was evaporated, the resultant residue was dissolved in water and the pH of the solution was adjusted to 7 by the addition of 1N HCl solution. The precipitated solid was collected by filtration, washed with water (2 mL) then diethyl ether (2 mL) and left to air dry to provide the title compound as a yellow solid (80 mg, 92%). LCMS (method B): RT=2.11 min, M+H+=412.

후처리

  1. temperatureAfter cooling to ambient temperature the solvent
  2. customwas evaporated
  3. dissolutionthe resultant residue was dissolved in water
  4. additionthe pH of the solution was adjusted to 7 by the addition of 1N HCl solution
  5. filtrationThe precipitated solid was collected by filtration
  6. washwashed with water (2 mL)
  7. waitdiethyl ether (2 mL) and left to air
  8. customdry

출처 및 근거

ORD 기록
ord-b096c9cd1ece4b55ac3e6d2e05f8b7c8
출처 데이터셋
uspto-grants-2010_12
특허 번호
US07855216B2

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