Triethylamine → HCID 10975521, 화합물

HRID 727433

반응식

HRID 727433 반응식
C([NH:9][CH2:10][C@@H:11]([C@H:16]([OH:18])[CH3:17])[C:12]([O:14]C)=[O:13])(=O)C1C=CC=CC=1.C(N(CC)CC)C>Cl>[NH2:9][CH2:10][C@@H:11]([C@H:16]([OH:18])[CH3:17])[C:12]([OH:14])=[O:13]

참가 물질

4

반응물 2

HCID 8471TriethylamineHCID 10060699(2S,3R)-methyl-2-benzamidomethyl-3-hydroxybutyrate

생성물 1

HCID 10975521HCID 10975521, 화합물수율 80%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

20.08 g (0.08 mole) of methyl (2S,3R)-2-(N-benzoyl amino)methyl-3-hydroxybutyrate were dissolved in 60.8 g of 12N-hydrochloric acid solution, refluxed with application of heat for 6 hours and cooled to room temperature, so that a solid was precipitated. After the solid was filtered, the filtrate was washed twice with 100 ml of toluene. Then a water phase was concentrated to a residue in vacuo. To this was added 250 ml of acetonitrile and further, under an ice water cooling, 0.08 g (0.08 mole) of triethylamine. The total solution was stirred overnight at room temperature to yield precipitates. The precipitates were filtered, washed with 200 ml of acetonitrile and dried in vacuo, thereby obtaining 8.51 g (0.06 mole) of (2S,3R)-2-aminomethyl-3-hydroxybutyric acid. Yield was 80%. This compound corresponded to that described in the Japanese published application Hei 2-134 349 according to an 1H-NMR spectrum analysis.

후처리

  1. temperaturerefluxed with application
  2. temperatureof heat for 6 hours
  3. customwas precipitated
  4. filtrationAfter the solid was filtered
  5. washthe filtrate was washed twice with 100 ml of toluene
  6. concentrationThen a water phase was concentrated to a residue in vacuo
  7. additionTo this was added 250 ml of acetonitrile
  8. customto yield
  9. customprecipitates
  10. filtrationThe precipitates were filtered
  11. washwashed with 200 ml of acetonitrile
  12. customdried in vacuo

출처 및 근거

ORD 기록
ord-04573850af834060bea86b2fadf1c5b5
출처 데이터셋
uspto-grants-1998_01
특허 번호
US05712388

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