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

HRID 69885노트

반응식

[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

참가 물질

반응물 4

HCID 313Hydrochloric Acid

HCID 3939Lithium Hydroxide

HCID 21899815MeOH tetrahydrofuran

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

생성물 1

HCID 64521193,5-Diamino-6-chloro-pyrazine acid수율 93%

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록: ord-671c1c7fb69541e4af32669088ce1d08
출처 데이터셋: uspto-grants-2014_09
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US08822497B2

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