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Water → HCID 66971245, 화합물

HRID 1361286
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HRID 1361286 반응식
[C:1]([N:8]1[CH2:12][C@@H:11]([N:13]=[N+]=[N-])[CH2:10][C@@H:9]1[CH2:16][CH:17]=[CH2:18])([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].CP(C)C.O>C1COCC1>[C:1]([N:8]1[CH2:12][C@H:11]([NH2:13])[CH2:10][C@@H:9]1[CH2:16][CH:17]=[CH2:18])([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 68983TrimethylphosphineHCID 86636639HCID 86636639, 화합물

생성물 1

HCID 66971245HCID 66971245, 화합물수율 70%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of (2S,4R)-1-Boc-2-allyl-4-azidopyrrolidine (450 mg, 1.78 mmol) prepared in Step B in THF was added dropwise trimethylphosphine (135 mg, 1.78 mmol). After the reaction mixture was stirred at rt for 5 h, water (0.03 ml) was added, and stirred for additional 20 min. The reaction mixture was concentrated in vacuo, extracted with EtOAc, washed with water and brine, and concentrated in vacuo. The residue was purified by column chromatography(eluent, MeOH/DCM=1/9) to give the title compound (280 mg, 70%).

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후처리

  1. stirringstirred for additional 20 min
  2. concentrationThe reaction mixture was concentrated in vacuo
  3. extractionextracted with EtOAc
  4. washwashed with water and brine
  5. concentrationconcentrated in vacuo
  6. customThe residue was purified by column chromatography(eluent, MeOH/DCM=1/9)

출처 및 근거

ORD 기록
ord-ce81ec8185fd4aef9da25c413392418c
출처 데이터셋
uspto-grants-2011_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07879852B2

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