Hydrochloric Acid → N-Methyl-N-[2-(5-chloro-2,3-dihydro-2-oxo-3-phenyl-3-benzofuranyl)acetyl]leucine

HRID 476575

반응식

HRID 476575 반응식
[OH-].[Na+].[CH3:3][NH:4][C@H:5]([C:10]([OH:12])=[O:11])[CH2:6][CH:7]([CH3:9])[CH3:8].[Cl:13][C:14]1[CH:15]=[CH:16][C:17]2[O:21][C:20](=[O:22])[C:19]([CH2:29][C:30](Cl)=[O:31])([C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=3)[C:18]=2[CH:33]=1.Cl>O.O1CCCC1>[CH3:3][N:4]([C:30](=[O:31])[CH2:29][C:19]1([C:23]2[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=2)[C:18]2[CH:33]=[C:14]([Cl:13])[CH:15]=[CH:16][C:17]=2[O:21][C:20]1=[O:22])[C@H:5]([C:10]([OH:12])=[O:11])[CH2:6][CH:7]([CH3:9])[CH3:8]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 14798Sodium Hydroxide2회HCID 2777993N-MethylleucineHCID 143034982-(5-Chloro-2,3-dihydro-2-oxo-3-phenyl-3-benzofuranyl)acetyl chloride

생성물 1

HCID 54373910N-Methyl-N-[2-(5-chloro-2,3-dihydro-2-oxo-3-phenyl-3-benzofuranyl)acetyl]leucine

시약·촉매·용매 2

HCID 962Water용매2회HCID 8028Tetrahydrofuran용매2회

반응 조건

온도
5 °C

실험 절차

0.9 g of sodium hydroxide is added to a solution of 3 g of N-methylleucine in 70 ml of water and 40 ml of tetrahydrofuran. The medium is then cooled to 5° C. and a solution of 7.3 g of 2-(5-chloro-2,3-dihydro-2-oxo-3-phenyl-3-benzofuranyl)acetyl chloride in 50 ml of tetrahydrofuran and a solution of 0.9 g of sodium hydroxide in 22.7 ml of water are then added simultaneously in small portions so as to maintain the pH at 12. The mixture is stirred for 3 hours at room temperature and 22.7 ml of N hydrochloric acid are added. The medium is concentrated and the precipitate obtained is filtered off and dissolved hot in an ethanol/methanol (50:50) mixture. The solution is filtered and the filtrate evaporated. A crystalline product is obtained.

후처리

  1. temperatureto maintain the pH at 12
  2. concentrationThe medium is concentrated
  3. customthe precipitate obtained
  4. filtrationis filtered off
  5. dissolutiondissolved hot in an ethanol/methanol (50:50) mixture
  6. filtrationThe solution is filtered
  7. customthe filtrate evaporated
  8. customA crystalline product is obtained

출처 및 근거

ORD 기록
ord-12927ed5c2344696bf9d6c183ec449d6
출처 데이터셋
uspto-grants-1989_12
특허 번호
US04885299

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