Water → HCID 136359197、化合物

HRID 1155541ノート

反応式

HRID 1155541 の反応式
Cl.[NH2:2][OH:3].O.[OH-].[Na+].[CH2:7]([NH:9][C:10]1[CH:15]=[C:14]([C:16](=O)[CH3:17])[CH:13]=[CH:12][N:11]=1)[CH3:8]>CO>[CH2:7]([NH:9][C:10]1[CH:15]=[C:14]([C:16](=[N:2][OH:3])[CH3:17])[CH:13]=[CH:12][N:11]=1)[CH3:8]

参加物

6

反応物 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 443297Hydroxyamine hydrochlorideHCID 131452661-(2-Ethylamino-4-pyridyl)-1-ethanone

生成物 1

HCID 136359197HCID 136359197、化合物収率 87%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a mixture of 7 g. (0.1 mole) of hydroxylamine hydrochloride in 40 ml. of water and 50 ml. of 2 N sodium hydroxide was added 11.5 g. (70 mmoles) of 1-(2-ethylamino-4-pyridyl)-1-ethanone, and the resulting mixture heated to boiling. Methanol was carefully added until the mixture became homogeneous. Heating was continued until the mixture became cloudy. The mixture was cooled and the resulting precipitate filtered, washed with water and dried. Recrystallization from toluene gave 10.9 g. (87%) of the desired product, m.p. 155°-156° C.

後処理

  1. additionTo a mixture of 7 g
  2. temperatureHeating
  3. temperatureThe mixture was cooled
  4. filtrationthe resulting precipitate filtered
  5. washwashed with water
  6. customdried
  7. customRecrystallization from toluene
  8. customgave 10.9 g

出典と根拠

ORDレコード
ord-326e57327d40407a9207cc1b20120c85
出典データセット
uspto-grants-1981_11
特許番号
US04302464

反応ノート

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