Hydrochloric Acid → HCID 15578596, 화합물

HRID 729015노트

반응식

HRID 729015 반응식
Cl.[NH2:2][CH2:3][CH2:4][C:5]([O:7][CH2:8][CH3:9])=[O:6].[CH3:10][O:11][C:12]1[CH:13]=[C:14]([CH:20]=[CH:21][CH:22]=1)[O:15][CH2:16][CH:17]1[O:19][CH2:18]1.[OH-].[Na+]>>[CH3:10][O:11][C:12]1[CH:13]=[C:14]([CH:20]=[CH:21][CH:22]=1)[O:15][CH2:16][CH:17]([OH:19])[CH2:18][NH:2][CH2:3][CH2:4][C:5]([O:7][CH2:8][CH3:9])=[O:6]

참가 물질

5

반응물 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 419889Ethyl 3-aminopropanoateHCID 129593782-[(3-methoxyphenoxy)methyl]oxirane

생성물 1

HCID 15578596HCID 15578596, 화합물

실험 절차

This compound was prepared in accordance with Example 1 using 7.6 g of the hydrochloride of ethyl 3-aminopropanoate, 4.5 g of 3-(3-methoxyphenoxy)-1,2-epoxypropane, and 2.0 g of NaOH. The crude product was washed with 150 ml of water and dissolved in 100 ml of water and 10 ml of 2-n HCl. This solution was extracted with ethyl acetate, treated with NaHCO3, and extracted with CH2Cl2. The organic layer was separated, dried over MgSO4, filtered and evaporated. Ethyl N-[3-(2-cyano-4-methoxyphenoxy)-2-hydroxypropyl]-3-aminopropanoate crystallized. Yield 1.2 g. Melting point 72° C. (base). The structure was determined by NMR.

후처리

  1. washThe crude product was washed with 150 ml of water
  2. dissolutiondissolved in 100 ml of water
  3. extractionThis solution was extracted with ethyl acetate
  4. additiontreated with NaHCO3
  5. extractionextracted with CH2Cl2
  6. customThe organic layer was separated
  7. dry with materialdried over MgSO4
  8. filtrationfiltered
  9. customevaporated
  10. customEthyl N-[3-(2-cyano-4-methoxyphenoxy)-2-hydroxypropyl]-3-aminopropanoate crystallized

출처 및 근거

ORD 기록
ord-4187494a97114343b795371f21d4d307
출처 데이터셋
uspto-grants-1991_09
특허 번호
US05051446

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