Hydrochloric Acid → (3aR,6aS)-Octahydrocyclopenta[c]pyrrol-5-ol--hydrogen chloride (1/1)

HRID 2367166노트

반응식

HRID 2367166 반응식
CC(OC([N:8]1[CH2:15][C@H:14]2[C@H:10]([CH2:11][CH:12]([OH:16])[CH2:13]2)[CH2:9]1)=O)(C)C.[ClH:17]>O1CCOCC1.ClCCCl.C(OCC)C>[CH2:11]1[CH:12]([OH:16])[CH2:13][C@@H:14]2[C@H:10]1[CH2:9][NH:8][CH2:15]2.[ClH:17]

참가 물질

6

반응물 2

HCID 313Hydrochloric AcidHCID 20753133(Meso-3aR,5r,6aS)-tert-butyl 5-hydroxyhexahydrocyclopenta[c]pyrrole-2(1H)-carboxylate

생성물 1

HCID 67281394(3aR,6aS)-Octahydrocyclopenta[c]pyrrol-5-ol--hydrogen chloride (1/1)

시약·촉매·용매 3

HCID 111,2-Dichloroethane용매HCID 3283Diethyl Ether용매HCID 312751,4-Dioxane용매2회

실험 절차

3.00 g (13.20 mmol) of tert-butyl (3aR,5r,6aS)-5-hydroxyhexahydrocyclopenta[c]pyrrole-2(1H)-carboxylate (see synthesis: WO 2006/108 059) are dissolved in 150 mL of a 2/1 mixture of dioxane and 1,2-dichloroethane. 30 mL (120 mmol) of a 4N solution of hydrogen chloride in dioxane are poured into the medium with stirring. After stirring for 3 hours at room temperature, the medium is concentrated to dryness and the product obtained in hydrochloride form is taken up in diethyl ether for organization of the salt. After filtering off and drying under reduced pressure, 1.745 g (81%) of the expected product are obtained in the form of a hygroscopic solid.

후처리

  1. stirringAfter stirring for 3 hours at room temperature
  2. concentrationthe medium is concentrated to dryness
  3. customthe product obtained in hydrochloride form
  4. filtrationAfter filtering off
  5. dry with materialdrying under reduced pressure, 1.745 g (81%) of the expected product
  6. customare obtained in the form of a hygroscopic solid

출처 및 근거

ORD 기록
ord-4d1494385ebc4c37be8a521a83e13e0f
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08697883B2

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