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Tetrahydrofuran → HCID 70014061, 화합물

HRID 1368760
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HRID 1368760 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:10][C@@H:9]1[C@H:11]([O:14][Si:15]([C:18]([CH3:21])([CH3:20])[CH3:19])([CH3:17])[CH3:16])[CH2:12][Cl:13])=[O:7])([CH3:4])([CH3:3])[CH3:2].[C:22]1([Mg]Cl)[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1.C1COCC1.[NH4+].[Cl-]>C1(C)C=CC=CC=1>[Si:15]([O:14][C@@H:11]([C@H:9]([NH:8][C:6]([O:5][C:1]([CH3:3])([CH3:2])[CH3:4])=[O:7])[CH2:10][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)[CH2:12][Cl:13])([C:18]([CH3:21])([CH3:19])[CH3:20])([CH3:16])[CH3:17]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 8028TetrahydrofuranHCID 25517Ammonium ChlorideHCID 11371084HCID 11371084, 화합물HCID 178478979HCID 178478979, 화합물

생성물 1

HCID 70014061HCID 70014061, 화합물수율 75%

시약·촉매·용매 1

HCID 1140Toluene용매

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온도
-78 °C

실험 절차

To a magnetically stirred solution of N-t-butyloxycarbonyl-2(R)-(1(S)-t-butyldimetylsilyloxy-2-chloroethyl)aziridine (36.0 mg, 0.107 mmol) in toluene was added copper bromide dimethyl sulfide complex (11.0 mg, 0.054 mmol) at rt under N2. The reaction mixture was cooled to −78° C. then treated with a 2 M solution of PhMgCl in THF (0.54 mL, 1.072 mmol). The resulting mixture was warmed to −20° C. and stirred overnight. The reaction mixture was treated with sat NH4Cl (4 mL) and extracted with EtOAc(5 mL×3). The combined organic layers were washed with brine (50 mL), dried over anhydrous magnesium sulfate, filtered, concentrated and column-chromatographed (3% EtAc in n-Hex) to provide 2(S)-t-butyldimetylsilyloxy-3(R)-(t-butyloxycarbonyl)amino-1-chloro-4-phenylbutane (33.5 mg) as a colorless oil.

후처리

  1. temperatureThe resulting mixture was warmed to −20° C.
  2. extractionextracted with EtOAc(5 mL×3)
  3. washThe combined organic layers were washed with brine (50 mL)
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customcolumn-chromatographed (3% EtAc in n-Hex)

출처 및 근거

ORD 기록
ord-13f4235db4994afbb606a13c157d7c0e
출처 데이터셋
uspto-grants-2003_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06573388B1

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