N,N'-Di-Boc-1H-pyrazole-1-carboximidamide → HCID 178454299, 화합물

HRID 1441380노트

반응식

HRID 1441380 반응식
[CH:1]1([NH:4][C:5]([C@H:7]2[CH2:11][CH2:10][CH2:9][N:8]2[C:12]2[CH:17]=[CH:16][C:15]([NH2:18])=[CH:14][CH:13]=2)=[O:6])[CH2:3][CH2:2]1.[C:19]([O:23][C:24](=[O:40])[NH:25]/[C:26](/N1C=CC=N1)=[N:27]/[C:28](=[O:34])[O:29][C:30]([CH3:33])([CH3:32])[CH3:31])([CH3:22])([CH3:21])[CH3:20]>C(Cl)Cl>[C:30]([O:29][C:28]([NH:27]/[C:26](/[NH:18][C:15]1[CH:14]=[CH:13][C:12]([N:8]2[CH2:9][CH2:10][CH2:11][C@@H:7]2[C:5]([NH:4][CH:1]2[CH2:2][CH2:3]2)=[O:6])=[CH:17][CH:16]=1)=[N:25]/[C:24]([O:23][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:40])=[O:34])([CH3:33])([CH3:32])[CH3:31]

참가 물질

4

반응물 2

HCID 6383521N,N'-Di-Boc-1H-pyrazole-1-carboximidamideHCID 68689756(R)-1-(4-Amino-phenyl)-pyrrolidine-2-carboxylic acid cyclopropylamide

생성물 1

HCID 178454299HCID 178454299, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

(R)-1-(4-Amino-phenyl)-pyrrolidine-2-carboxylic acid cyclopropylamide (Method 61; 1.2 g, 4.9 mmol) in DCM (60 ml) was added di-tert-butyl[(Z)-1H-pyrazol-1-ylmethylylidene]biscarbamate (1.9 g, 6.1 mmol) in one portion. The reaction was stirred overnight before removal of the solvent in vacuo. The residue was purified via column chromatography eluting with 20% ethylactetate/isohexane, 50% EtOAc/isohexane and finally 100% EtOAc. The title compound was obtained as a white foam (2.0 g, 81%). NMR (299.954 MHz, CDCl3) 11.63 (s, 1H), 10.09 (s, 1H), 7.60 (s, 1H), 7.40 (d, 2H), 6.45 (m, 3H), 3.92 (t, 1H), 3.59 (t, 1H), 3.19 (q, 1H), 2.69 (m, 1H), 2.29-2.22 (m, 2H), 2.03-1.84 (m, 2H), 1.53 (s, 9H), 1.49 (s, 9H), 0.80-0.68 (m, 2H), 0.44-0.32 (m, 2H); m/z 488.

후처리

  1. customThe residue was purified via column chromatography
  2. washeluting with 20% ethylactetate/isohexane, 50% EtOAc/isohexane and finally 100% EtOAc

출처 및 근거

ORD 기록
ord-79686abf1e7840c9a0d4129d9d6b1ead
출처 데이터셋
uspto-grants-2010_02
특허 번호
US07655652B2

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