Diisopropylethylamine → 1-Pyrimidin-2-yl-piperidine-4-carboxylic acid N'-(3-methyl-butyryl)-hydrazide

HRID 6913

반응식

HRID 6913 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.[OH2:16].ON1C2C=[CH:24][CH:25]=[CH:26][C:21]=2[N:20]=[N:19]1.Cl.[CH3:28]N(C)CCCN=C=NCC.C(N(C(C)C)CC)(C)C>ClCCl>[CH3:28][CH:25]([CH3:24])[CH2:26][C:21]([NH:20][NH:19][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:16]

참가 물질

6

반응물 4

HCID 81531DiisopropylethylamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 27672671-(Pyrimidin-2-yl)piperidine-4-carboxylic acidHCID 27960291-Hydroxybenzotriazole hydrate

생성물 1

HCID 235440671-Pyrimidin-2-yl-piperidine-4-carboxylic acid N'-(3-methyl-butyryl)-hydrazide수율 46.4%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

The residue was added to a mixture of 1-pyrimidin-2-yl-piperidine-4-carboxylic acid (6.6 g, 31.7 mmol) (see reference U.S. Pat. No. 4,826,843), 1-hydroxybenzotriazole hydrate (4.28 g, 31.7 mmol) and 1-(3-dimethylaminopropyl-3-ethylcarbodiimide hydrochloride (6.09 g, 31.7 mmol) in dichloromethane (50 ml). Diisopropylethylamine (17 ml, 95 mmol) was added and the mixture was stirred for 3 days. The solvent was evaporated and the residue was triturated with water and then with diethyl ether to give the title compound as a white solid (4.49 g).

후처리

  1. customThe solvent was evaporated
  2. customthe residue was triturated with water

출처 및 근거

ORD 기록
ord-4c0cc20436e440c9a6f5ae1c9ddc1270
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07084145B2

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