Hydrochloric Acid → (3R)-ethyl 2-amino-3-ethyl-5-methylnon-8-enoate hydrochloride

HRID 523190노트

반응식

HRID 523190 반응식
C1(C(=[N:14][CH:15]([C@H:21]([CH2:29][CH3:30])[CH2:22][CH:23]([CH3:28])[CH2:24][CH2:25][CH:26]=[CH2:27])[C:16]([O:18][CH2:19][CH3:20])=[O:17])C2C=CC=CC=2)C=CC=CC=1.[ClH:31]>C(OCC)C>[ClH:31].[NH2:14][CH:15]([C@H:21]([CH2:29][CH3:30])[CH2:22][CH:23]([CH3:28])[CH2:24][CH2:25][CH:26]=[CH2:27])[C:16]([O:18][CH2:19][CH3:20])=[O:17]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 86683257(3R)-ethyl 2-(diphenylmethyleneamino)-3-ethyl-5-methylnon-8-enoate

생성물 1

HCID 86683258(3R)-ethyl 2-amino-3-ethyl-5-methylnon-8-enoate hydrochloride수율 62.4%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

A solution of (3R)-ethyl 2-(diphenylmethyleneamino)-3-ethyl-5-methylnon-8-enoate (7.00 g, 17.3 mmole) in diethyl ether (20 mL) was added aqueous 1.5 N HCl solutions (100 mL) and the reaction mass was stirred at room temperature overnight. The reaction mass was washed with diethyl ether (100 mL). The aqueous solution was basified using saturated sodium bicarbonate solution and extracted with ethyl acetate (100 mL×3). The combined organic layers were dried over anhydrous Na2SO4; filtered; then concentrated under reduced pressure to get crude compound (2.6 g, 62.4%). The crude compound was taken to the next step without further purification. MS: MS m/z 242.4 (M++1).

후처리

  1. washThe reaction mass was washed with diethyl ether (100 mL)
  2. extractionextracted with ethyl acetate (100 mL×3)
  3. dry with materialThe combined organic layers were dried over anhydrous Na2SO4
  4. filtrationfiltered
  5. concentrationthen concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-67a621aae5d143ffb991fb448b27d6e6
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09334279B2

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