Diisopropylethylamine → HCID 71092810, 화합물

HRID 1522087노트

반응식

HRID 1522087 반응식
[Cl:1][C:2]1[C:3]([NH2:9])=[N:4][CH:5]=[N:6][C:7]=1Cl.[NH2:10][CH2:11][CH:12]1[CH2:17][CH2:16][N:15]([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[CH2:14][CH2:13]1.C(N(CC)C(C)C)(C)C>CN1C(=O)CCC1>[NH2:9][C:3]1[N:4]=[CH:5][N:6]=[C:7]([NH:10][CH2:11][CH:12]2[CH2:17][CH2:16][N:15]([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[CH2:14][CH2:13]2)[C:2]=1[Cl:1]

참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 7368171-Boc-4-(aminomethyl)piperidineHCID 242192625,6-Dichloro-pyrimidin-4-ylamine

생성물 1

HCID 71092810HCID 71092810, 화합물

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

실험 절차

Into a 10-mL vial was placed 5,6-dichloropyrimidin-4-amine (250.00 mg; 1.52 mmol), tert-butyl 4-(aminomethyl)piperidine-1-carboxylate (653.40 mg; 3.05 mmol), and N,N-diisopropylethylamine (1.01 ml; 6.10 mmol) suspended in NMP (2.50 ml). The reaction mixture was run in the microwave at 150° C. for 2 hours. The reaction mixture was allowed to cool to rt. The mixture was purified using Biotage column chromatography eluting from 50-100% EtOAc/Hexanes. Fractions containing the desired product were combined and concentrated under reduced pressure to afford tert-butyl 4-{[(6-amino-5-chloropyrimidin-4-yl)amino]methyl}piperidine-1-carboxylate as a yellow viscous oil.

후처리

  1. customThe mixture was purified
  2. washeluting from 50-100% EtOAc/Hexanes
  3. additionFractions containing the desired product
  4. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-a88b0fd9e26b458ca627e84b7842006a
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09073947B2

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