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

HRID 2264900ノート

反応式

HRID 2264900 の反応式
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]

参加物

3

反応物 1

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

生成物 1

HCID 59596445HCID 59596445、化合物収率 97.3%

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

反応条件

温度
65 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b096c9cd1ece4b55ac3e6d2e05f8b7c8
出典データセット
uspto-grants-2010_12
特許番号
US07855216B2

反応ノート

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