Methanesulfonic Acid → 2-(3,5-Dichlorophenyl)-tetrahydro-imidazo[1,5-a]pyrazine-1,3-dione

HRID 49977

반응식

HRID 49977 반응식
CS(O)(=O)=O.C(OC([N:13]1[CH2:18][CH2:17][N:16]2[C:19](=[O:31])[N:20]([C:23]3[CH:28]=[C:27]([Cl:29])[CH:26]=[C:25]([Cl:30])[CH:24]=3)[C:21](=[O:22])[CH:15]2[CH2:14]1)=O)(C)(C)C>C(Cl)Cl>[Cl:29][C:27]1[CH:28]=[C:23]([N:20]2[C:21](=[O:22])[CH:15]3[CH2:14][NH:13][CH2:18][CH2:17][N:16]3[C:19]2=[O:31])[CH:24]=[C:25]([Cl:30])[CH:26]=1

참가 물질

4

반응물 2

HCID 6395Methanesulfonic AcidHCID 224792022-(3,5-Dichlorophenyl)-1,3-dioxo-hexahydro-imidazo[1,5-a]pyrazine-7-carboxylic Acid Tert-Butyl Ester

생성물 1

HCID 213010012-(3,5-Dichlorophenyl)-tetrahydro-imidazo[1,5-a]pyrazine-1,3-dione수율 86.6%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Methanesulfonic acid (2.1 mL, 32.7 mmol) was added to an ice-cold solution of 2-(3,5-Dichlorophenyl)-1,3-dioxo-hexahydro-imidazo[1,5-a]pyrazine-7-carboxylic acid tert-butyl ester (2.62 g, 6.54 mmol, Prep. 18) in methylene chloride (50 mL). After 1 h at RT, TEA (5 mL, 36 mmol) was added. The reaction mixture was washed twice with water, dried over sodium sulfate and concentrated in vacuo to yield the above compound (1.7 g) as a white solid. Mp=134° C. (crystallized from diethyl ether).

후처리

  1. washThe reaction mixture was washed twice with water
  2. dry with materialdried over sodium sulfate
  3. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-8a0b8336ae4c49f1b62ba2ba780e4fce
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06710064B2

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