Triphenylphosphine → HCID 86705166, 화합물

HRID 2401260노트

반응식

HRID 2401260 반응식
C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.N(C(OCC)=O)=NC(OCC)=O.O[CH2:33][C@@H:34]([NH:38][C:39]([NH:41][C:42]1[CH:43]=[N:44][C:45]([C:48]([F:51])([F:50])[F:49])=[CH:46][CH:47]=1)=[O:40])[CH:35]([CH3:37])[CH3:36]>C1COCC1>[CH3:36][CH:35]([C@H:34]1[CH2:33][N:41]([C:42]2[CH:43]=[N:44][C:45]([C:48]([F:51])([F:50])[F:49])=[CH:46][CH:47]=2)[C:39](=[O:40])[NH:38]1)[CH3:37]

참가 물질

5

반응물 3

HCID 11776TriphenylphosphineHCID 220568ethyl N-ethoxycarbonyliminocarbamateHCID 86705165HCID 86705165, 화합물

생성물 1

HCID 86705166HCID 86705166, 화합물수율 83.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Triphenylphosphine (770 mg) and diethyl azodicarboxylate (2.2 M solution in toluene, 1.3 mL) were added to a solution of 1-[(2S)-1-hydroxy-3-methylbutan-2-yl]-3-[6-(trifluoromethyl)pyridin-3-yl]urea (640 mg) in THF (10 mL), and the mixture was stirred at room temperature for 1 hr. The reaction mixture was concentrated under reduced pressure, the residue was purified by column chromatography (silica gel cartridge and NH silica gel cartridge, hexane/ethyl acetate), and the resulting solid was washed with isopropyl ether to afford the title compound (500 mg). This product contained by-products originating in reaction reagents.

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. customthe residue was purified by column chromatography (silica gel cartridge and NH silica gel cartridge, hexane/ethyl acetate)
  3. washthe resulting solid was washed with isopropyl ether

출처 및 근거

ORD 기록
ord-faaebe45a57142d3973c21322a5094c9
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08796272B2

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