Hydrochloric Acid → 3,5-Diamino-6-chloro-pyrazine acid

反応式

[NH2:1][C:2]1[C:3](NC(OC)=O)=[N:4][C:5]([Cl:9])=[C:6]([NH2:8])[N:7]=1.[Li+].[OH-:16].Cl.C1[CH2:22][O:21]CC1.CO>>[NH2:1][C:2]1[C:3]([C:22]([OH:21])=[O:16])=[N:4][C:5]([Cl:9])=[C:6]([NH2:8])[N:7]=1

参加物

反応物 4

HCID 313Hydrochloric Acid

HCID 3939Lithium Hydroxide

HCID 21899815MeOH tetrahydrofuran

HCID 86669184Methyl 3,5-diamino-6-chloropyrazine-2-carbamate

生成物 1

HCID 64521193,5-Diamino-6-chloro-pyrazine acid収率 93%

実験手順

To a solution of methyl 3,5-diamino-6-chloropyrazine-2-carbamate (5 g, 0.025 mols) in 2:1 THF/MeOH (90 mL) was added 1M LiOH (62 mL, 0.062 mols). After the reaction was stirred at r.t. 72 hrs, 1N HCl (62 mL, 0.062 mols) was added. The reaction was filtered and washed with water (3×10 mL) to give 3,5-diamino-6-chloropyrazine-2-carboxylic acid as white solid 4.3 g (93% yield). LCMS (m/z): 189.1 (MH+); LC Rt=1.05 min.

後処理

filtrationThe reaction was filtered
washwashed with water (3×10 mL)

出典と根拠

ORDレコード: ord-671c1c7fb69541e4af32669088ce1d08
出典データセット: uspto-grants-2014_09
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US08822497B2

反応ノート

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