(+-)-Methionine → HCID 178515872、化合物

HRID 2120273

反応式

HRID 2120273 の反応式
NC(C(O)=O)CCSC.C[O:11][C:12]1[CH:17]=[CH:16][C:15]([C:18]2[CH:22]=[CH:21][NH:20][N:19]=2)=[CH:14][CH:13]=1.CS(O)(=O)=O.[OH-].[Na+]>O>[NH:20]1[CH:21]=[CH:22][C:18]([C:15]2[CH:16]=[CH:17][C:12]([OH:11])=[CH:13][CH:14]=2)=[N:19]1

参加物

6

反応物 4

HCID 876(+-)-MethionineHCID 6395Methanesulfonic AcidHCID 14798Sodium HydroxideHCID 178488674HCID 178488674、化合物

生成物 1

HCID 178515872HCID 178515872、化合物収率 104.4%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
50 °C

実験手順

To a round-bottomed flask was added D,L-methionine (1.19 g, 7.96 mmol), 3-(4-methoxyphenyl)-pyrazole (990 mg, 5.68 mmol), and methanesulfonic acid (23 ml). The resulting solution was heated to about 50° C. for about forty-eight hours, and was then allowed to cool to room temperature and poured into water. The pH of the solution was adjusted to about 7 with 5 N sodium hydroxide, and was then extracted with ethyl acetate. The organic extracts were dried over magnesium sulfate, filtered, and concentrated in vacuo to afford 950 mg of a white solid which was determined to be about 95% pure by NMR. This material was subsequently employed directly without further purification.

後処理

  1. temperatureto cool to room temperature
  2. extractionwas then extracted with ethyl acetate
  3. dry with materialThe organic extracts were dried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-c350c59d444f40a9ae5cfd31ef20114d
出典データセット
uspto-grants-2004_02
特許番号
US06689888B2

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