Hydrazine hydrate (1:1) → 1-(Pyridin-2-yl)piperidine-4-carbohydrazide

HRID 269734ノート

反応式

HRID 269734 の反応式
C([O:3][C:4]([CH:6]1[CH2:11][CH2:10][N:9]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][N:13]=2)[CH2:8][CH2:7]1)=O)C.O.[NH2:19][NH2:20]>CO>[N:9]1([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][N:13]=2)[CH2:10][CH2:11][CH:6]([C:4]([NH:19][NH2:20])=[O:3])[CH2:7][CH2:8]1

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)2 回HCID 38156184-Piperidinecarboxylic acid, 1-(2-pyridinyl)-, ethyl ester

生成物 1

HCID 235440481-(Pyridin-2-yl)piperidine-4-carbohydrazide

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

3,4,5,6-Tetrahydro-2H-[1,2′]bipyridinyl-4-carboxylic acid ethyl ester (35 g, 150 mmol) (see reference Farmaco, 1993, 48(10), 1439) was dissolved in methanol (700 mL) containing hydrazine hydrate (34 mL, 150 mmol) and was heated under reflux for 18 hours. After this time, more hydrazine hydrate (22.7 mL, 100 mmol) was added and the mixture stirred for a further 18 hours. The mixture was cooled to room temperature and evaporated under reduced pressure. The solid formed was triturated with ethyl acetate to give the title compound as a white solid.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 18 hours
  3. customevaporated under reduced pressure
  4. customThe solid formed
  5. customwas triturated with ethyl acetate

出典と根拠

ORDレコード
ord-91b6afd42fe54328a546719c646703e3
出典データセット
uspto-grants-2008_11
特許番号
US07449462B2

反応ノート

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