Butyrohydrazide → 1-Pyrimidin-2-yl-piperidine-4-carboxylic acid N'-butyryl-hydrazide

HRID 6911

反応式

HRID 6911 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[N:3][C:2]=1[N:7]1[CH2:12][CH2:11][CH:10]([C:13]([OH:15])=O)[CH2:9][CH2:8]1.O.ON1C2C=CC=CC=2N=N1.Cl.CN(C)CCCN=C=NCC.[C:39]([NH:44][NH2:45])(=[O:43])[CH2:40][CH2:41][CH3:42]>ClCCl.C(=O)([O-])O.[Na+]>[C:39]([NH:44][NH:45][C:13]([CH:10]1[CH2:9][CH2:8][N:7]([C:2]2[N:1]=[CH:6][CH:5]=[CH:4][N:3]=2)[CH2:12][CH2:11]1)=[O:15])(=[O:43])[CH2:40][CH2:41][CH3:42]

参加物

7

反応物 4

HCID 77079ButyrohydrazideHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 27672671-(Pyrimidin-2-yl)piperidine-4-carboxylic acidHCID 27960291-Hydroxybenzotriazole hydrate

生成物 1

HCID 235440691-Pyrimidin-2-yl-piperidine-4-carboxylic acid N'-butyryl-hydrazide収率 62%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒2 回HCID 516892Sodium Bicarbonate溶媒

実験手順

A mixture of 1-pyrimidin-2-yl-piperidine-4-carboxylic acid (3.0 g, 14.5 mmol)(see reference U.S. Pat. No. 4,826,843), 1-hydroxybenzotriazole hydrate (1.96 g, 14.5 mmol) and 1-(3-dimethylaminopropyl-3-ethylcarbodiimide hydrochloride (2.78 g, 14.5 mmol) in dichloromethane (100 ml) was stirred for 10 minutes. Butyric acid hydrazide (1.78 g, 17.4 mmol) was added and the reaction mixture was stirred under a nitrogen atmosphere for 18 hours. The reaction mixture was diluted with dichloromethane (100 ml) and sodium hydrogen carbonate solution was added. The reaction mixture was concentrated under reduced pressure and the solid formed was isolated by filtration. The material obtained was dried under vacuum at 40° C. to give the title compound (2.62 g).

後処理

  1. additionwas added
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. customthe solid formed
  4. customwas isolated by filtration
  5. customThe material obtained
  6. customwas dried under vacuum at 40° C.

出典と根拠

ORDレコード
ord-4e299013dbfd48c1bf2a6e7afd13ee69
出典データセット
uspto-grants-2006_08
特許番号
US07084145B2

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