(+-)-Methionine → HCID 178515872, 화합물

HRID 2120273

반응식

HRID 2120273 반응식
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

참가 물질

6

반응물 4

HCID 876(+-)-MethionineHCID 6395Methanesulfonic AcidHCID 14798Sodium HydroxideHCID 178488674HCID 178488674, 화합물

생성물 1

HCID 178515872HCID 178515872, 화합물수율 104.4%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
50 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c350c59d444f40a9ae5cfd31ef20114d
출처 데이터셋
uspto-grants-2004_02
특허 번호
US06689888B2

연결된 노트

불러오는 중…