对甲氧基苯异氰酸酯 → Tert-butyl 4-(4-methoxyphenylcarbamoyl)-3-((pyridin-3-ylamino)methyl)piperazine-1-carboxylate

HRID 70233

反应方程式

HRID 70233 反应方程式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([N:9]=[C:10]=[O:11])=[CH:5][CH:4]=1.[N:12]1[CH:17]=[CH:16][CH:15]=[C:14]([NH:18][CH2:19][CH:20]2[NH:25][CH2:24][CH2:23][N:22]([C:26]([O:28][C:29]([CH3:32])([CH3:31])[CH3:30])=[O:27])[CH2:21]2)[CH:13]=1>C(Cl)Cl>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([NH:9][C:10]([N:25]2[CH2:24][CH2:23][N:22]([C:26]([O:28][C:29]([CH3:30])([CH3:31])[CH3:32])=[O:27])[CH2:21][CH:20]2[CH2:19][NH:18][C:14]2[CH:13]=[N:12][CH:17]=[CH:16][CH:15]=2)=[O:11])=[CH:7][CH:8]=1

参与物

4

反应物 2

HCID 79443对甲氧基苯异氰酸酯HCID 59671589Tert-butyl 3-((pyridin-3-ylamino)methyl)piperazine-1-carboxylate

产物 1

HCID 59671481Tert-butyl 4-(4-methoxyphenylcarbamoyl)-3-((pyridin-3-ylamino)methyl)piperazine-1-carboxylate

试剂、催化剂与溶剂 1

HCID 6344二氯甲烷溶剂

实验过程

4-Methoxyphenyl isocyanate (85 mg, 0.567 mmol) was added to a solution of tert-butyl 3-((pyridin-3-ylamino)methyl)piperazine-1-carboxylate (166 mg, 0.567 mmol) in CH2Cl2 (4 mL). After 1 h, the reaction mixture was concentrated under reduced pressure, and the material was purified by HPLC (10 to 90% MeCN/0.1% TFA in H2O/0.1% TFA gradient). This gave 81.7 mg (26%) of the TFA salt of the title compound as a white solid. LC-MS: RT=5.29 min, [M+H]+=442.2.

后处理

  1. concentrationthe reaction mixture was concentrated under reduced pressure
  2. customthe material was purified by HPLC (10 to 90% MeCN/0.1% TFA in H2O/0.1% TFA gradient)

来源与证据

ORD记录
ord-1777fc157d484a21a8c75ed44cbaf506
来源数据集
uspto-grants-2014_09
专利号
US08822472B2

关联笔记

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