Hydrochloric Acid → Methyl 2-amino-3-(pyrazine-2-carboxamido)benzoate

HRID 520446ノート

反応式

HRID 520446 の反応式
Cl.C(OC([N:9](C(OC(C)(C)C)=O)[C:10]1[C:19]([NH:20][C:21]([C:23]2[CH:28]=[N:27][CH:26]=[CH:25][N:24]=2)=[O:22])=[CH:18][CH:17]=[CH:16][C:11]=1[C:12]([O:14][CH3:15])=[O:13])=O)(C)(C)C>CO>[NH2:9][C:10]1[C:19]([NH:20][C:21]([C:23]2[CH:28]=[N:27][CH:26]=[CH:25][N:24]=2)=[O:22])=[CH:18][CH:17]=[CH:16][C:11]=1[C:12]([O:14][CH3:15])=[O:13]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 58552825Methyl 2-(bis-(tert-butoxycarbonyl)amino)-3-(pyrazine-2-carboxamido)benzoate

生成物 1

HCID 58552889Methyl 2-amino-3-(pyrazine-2-carboxamido)benzoate収率 85.3%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

HCl gas was bubbled through a solution of methyl 2-(bis-(tert-butoxycarbonyl)amino)-3-(pyrazine-2-carboxamido)benzoate 14 (2.8 g, 5.9 mmol) in MeOH (50 ml) for 2 h. The volatiles were removed in vacuo and H2O (20 mL) was added. The pH was adjusted to 7 using aq NaOH and the resulting precipitate was collected by filtration, rinsed with H2O, and dried under vacuum to give 15 (1.37 g, 85% yield).

後処理

  1. customThe volatiles were removed in vacuo and H2O (20 mL)
  2. additionwas added
  3. filtrationthe resulting precipitate was collected by filtration
  4. washrinsed with H2O
  5. customdried under vacuum

出典と根拠

ORDレコード
ord-ae83657fa39745ff91cb120e5eb5db9e
出典データセット
uspto-grants-2016_05
特許番号
US09326986B2

反応ノート

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