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Hydrochloric Acid → (S)-t-Butyl 2-((hydroxyimino)methyl)pyrrolidine-1-carboxylate

HRID 710030
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반응식

HRID 710030 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:12][CH2:11][CH2:10][C@H:9]1[CH:13]=O)=[O:7])([CH3:4])([CH3:3])[CH3:2].Cl.[NH2:16][OH:17].Cl>N1C=CC=CC=1>[OH:17][N:16]=[CH:13][C@@H:9]1[CH2:10][CH2:11][CH2:12][N:8]1[C:6]([O:5][C:1]([CH3:4])([CH3:3])[CH3:2])=[O:7]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 443297Hydroxyamine hydrochlorideHCID 2734674tert-butyl (2S)-2-formylpyrrolidine-1-carboxylate

생성물 1

HCID 86706742(S)-t-Butyl 2-((hydroxyimino)methyl)pyrrolidine-1-carboxylate수율 90.4%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

To a solution of (S)-t-butyl-2-formylpyrrolidine-1-carboxylate (40.94 g) in pyridine (411 mL), hydroxylamine monohydrochloride (28.56 g) was added at 0° C. and the mixture was stirred at room temperature for 17 hours. The reaction mixture was added to a mixture of AcOE (1.5 L) and hydrochloric acid (2 L, 3.0 N). The organic layer was separated, washed with saturated aqueous sodium bicarbonate (1 L), dried (MgSO4), filtered and concentrated to give the titled compound (39.78 g, colorless solid.)

후처리

  1. customThe organic layer was separated
  2. washwashed with saturated aqueous sodium bicarbonate (1 L)
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-5c0f90933b1e4bd984f338bc22ecc4e6
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09181229B2

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