Ethyl Acetate → HCID 178419928、化合物

HRID 2264209ノート

反応式

HRID 2264209 の反応式
[O:1]1[CH:5]=[CH:4][N:3]=[C:2]1[C:6]1[C:11]([C:12]2[CH:17]=[CH:16][N:15]=[CH:14][CH:13]=2)=[CH:10][C:9]([NH2:18])=[C:8]([NH2:19])[N:7]=1.[CH2:20](OC(OCC)OCC)C.[OH-].[Na+].C(OCC)(=O)C>C(O)(=O)C>[O:1]1[CH:5]=[CH:4][N:3]=[C:2]1[C:6]1[N:7]=[C:8]2[NH:19][CH:20]=[N:18][C:9]2=[CH:10][C:11]=1[C:12]1[CH:17]=[CH:16][N:15]=[CH:14][CH:13]=1

参加物

6

反応物 4

HCID 8857Ethyl AcetateHCID 14798Sodium HydroxideHCID 31214Ethyl orthoformateHCID 59595986HCID 59595986、化合物2 回

生成物 1

HCID 178419928HCID 178419928、化合物収率 49%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
140 °C

実験手順

A mixture of 2-(1,3-oxazol-2-yl)-3,4′-bipyridine-5,6-diamine (Intermediate 10, 0.100 g, 0.39 mmol) and triethylorthoformate (0.117 g, 0.79 mmol) in glacial acetic acid (2 mL) was heated in a sealed tube to 140° C. After stirring for 2 hours, the mixture was cooled and taken to pH 7 with 6N aqueous sodium hydroxide solution. Ethyl acetate was added to the mixture and, after stirring for 30 minutes, the separated solid was filtered, washed with diethyl ether and dried in vacuo to give the title compound (0.047 g, 49%) as an off-white solid.

後処理

  1. temperaturethe mixture was cooled
  2. stirringafter stirring for 30 minutes
  3. filtrationthe separated solid was filtered
  4. washwashed with diethyl ether
  5. customdried in vacuo

出典と根拠

ORDレコード
ord-575934924e984483af34fa8dd6ef9788
出典データセット
uspto-grants-2010_12
特許番号
US07855202B2

反応ノート

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