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

HRID 49977

反応式

HRID 49977 の反応式
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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-8a0b8336ae4c49f1b62ba2ba780e4fce
出典データセット
uspto-grants-2004_03
特許番号
US06710064B2

関連ノート

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