Hydrochloric Acid → 4-Oxo-hexahydro-pyrrolo[1,2-a]pyrazine-2,6-dicarboxylic acid 2-methyl ester

HRID 417446노트

반응식

HRID 417446 반응식
O.[OH-].[Li+].[CH3:4][O:5][C:6]([N:8]1[CH2:13][C:12](=[O:14])[N:11]2[CH:15]([C:18]([O:20]CC)=[O:19])[CH2:16][CH2:17][CH:10]2[CH2:9]1)=[O:7].Cl>O.CO.O1CCCC1>[CH3:4][O:5][C:6]([N:8]1[CH2:13][C:12](=[O:14])[N:11]2[CH:15]([C:18]([OH:20])=[O:19])[CH2:16][CH2:17][CH:10]2[CH2:9]1)=[O:7]

참가 물질

7

반응물 3

HCID 313Hydrochloric AcidHCID 168937Lithium hydroxide, monohydrateHCID 666205494-Oxo-hexahydro-pyrrolo[1,2-a]pyrazine-2,6-dicarboxylic acid 6-ethyl ester 2-methyl ester

생성물 1

HCID 666208694-Oxo-hexahydro-pyrrolo[1,2-a]pyrazine-2,6-dicarboxylic acid 2-methyl ester수율 100%

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

A solution of lithium hydroxide monohydrate (16.8 mg, 0.38 mmol) in water (0.5 mL) was added to a solution of 4-oxo-hexahydro-pyrrolo[1,2-a]pyrazine-2,6-dicarboxylic acid 6-ethyl ester 2-methyl ester (86 mg, 0.32 mmol) in methanol (1 mL) and tetrahydrofuran (1 mL). After 2 hours, an aqueous solution of hydrogen chloride (1N, 0.41 mL, 0.41 mmol) was added and the organic solvents were removed under reduced pressure. The resulting aqueous solution was lyophilized for 16 hours to give 4-oxo-hexahydro-pyrrolo[1,2-a]pyrazine-2,6-dicarboxylic acid 2-methyl ester. A yield of 100% was assumed for the subsequent step. C10H14N2O5 calculated 242.1, observed [M+1]+ 242.9, [M+1]− 241.1; rt=1.54 min.

후처리

  1. customthe organic solvents were removed under reduced pressure
  2. waitThe resulting aqueous solution was lyophilized for 16 hours

출처 및 근거

ORD 기록
ord-1b90342d5e8e43d88a3afc094ba23d3d
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08088368B2

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