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

HRID 6911

반응식

HRID 6911 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 6344Dichloromethane용매2회HCID 516892Sodium Bicarbonate용매

실험 절차

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).

후처리

  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.

출처 및 근거

ORD 기록
ord-4e299013dbfd48c1bf2a6e7afd13ee69
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07084145B2

연결된 노트

불러오는 중…