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Hydrochloric Acid → (2S,3S)-2-Amino-3-methyl-1-(3,3,4,4-tetrafluoro-pyrrolidin-1-yl)-pentan-1-one Hydrochloride

HRID 2414457
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HRID 2414457 반응식
C(OC(=O)[NH:7][C@H:8]([C:13]([N:15]1[CH2:19][C:18]([F:21])([F:20])[C:17]([F:23])([F:22])[CH2:16]1)=[O:14])[C@@H:9]([CH3:12])[CH2:10][CH3:11])(C)(C)C.[ClH:25]>C(OCC)(=O)C>[ClH:25].[NH2:7][C@@H:8]([C@@H:9]([CH3:12])[CH2:10][CH3:11])[C:13]([N:15]1[CH2:19][C:18]([F:20])([F:21])[C:17]([F:23])([F:22])[CH2:16]1)=[O:14]
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참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 86590627[(1S,2S)-2-Methyl-1-(3,3,4,4-tetrafluoro-pyrrolidine-1-carbonyl)-butyl]-carbamic acid tert-butyl ester

생성물 1

HCID 9882539(2S,3S)-2-Amino-3-methyl-1-(3,3,4,4-tetrafluoro-pyrrolidin-1-yl)-pentan-1-one Hydrochloride

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

반응 조건

온도
0 °C

실험 절차

[(1S,2S)-2-Methyl-1-(3,3,4,4-tetrafluoro-pyrrolidine-1-carbonyl)-butyl]-carbamic acid tert-butyl ester (200 mg, 0.56 mmol) was dissolved in ethyl acetate (4 mL), cooled to about 0° C. and treated with gaseous hydrochloric acid for about 1 minute. After about 15 minutes at about 0° C. and about 30 minutes at room temperature, the mixture was concentrated to dryness and the solid was triturated with hexane, collected and dried under vacuum overnight (124 mg, 76%, melting point: greater than 250° C.).

후처리

  1. concentrationabout 30 minutes at room temperature, the mixture was concentrated to dryness
  2. customthe solid was triturated with hexane
  3. customcollected
  4. customdried under vacuum overnight (124 mg, 76%, melting point: greater than 250° C.)

출처 및 근거

ORD 기록
ord-71d03654bdd34c399f37660aaa74d91a
출처 데이터셋
uspto-grants-2004_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06812350B2

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