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Hydroxyamine hydrochloride → HCID 178452026, 화합물

HRID 1040413
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HRID 1040413 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:12][CH2:11][C@@H:10]([C:13]#[N:14])[CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].Cl.[NH2:16][OH:17].C([O-])(O)=O.[Na+]>CO>[C:1]([O:5][C:6]([N:8]1[CH2:12][CH2:11][C@@H:10]([C:13](=[NH:14])[NH:16][OH:17])[CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 443297Hydroxyamine hydrochlorideHCID 516892Sodium BicarbonateHCID 7018344(R)-1-Boc-3-cyanopyrrolidine

생성물 1

HCID 178452026HCID 178452026, 화합물수율 77.8%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

(R)-3-Cyano-pyrrolidine-1-carboxylic acid tert-butyl ester (1.02 g, 5.2 mmol), hydroxylamine hydrochloride (396 mg, 5.7 mmol) and NaHCO3 (487 mg, 5.8 mmol) were added to MeOH (12 mL) and the solution was heated to reflux. After 4 h, the reaction was concentrated in vacuo. The residue was partitioned between EtOAc and brine. The layers were separated and the organic layer was dried over Na2SO4, filtered and concentrated to yield 927 mg of crude (R)-3-(N-hydroxycarbamimidoyl)-pyrrolidine-1-carboxylic acid tert-butyl ester as a yellow foam.

후처리

  1. temperaturethe solution was heated to reflux
  2. concentrationthe reaction was concentrated in vacuo
  3. customThe residue was partitioned between EtOAc and brine
  4. customThe layers were separated
  5. dry with materialthe organic layer was dried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-748e87e2859e41a5bc939bcb0dcfc6f2
출처 데이터셋
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08552205B2

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