Triphenylphosphine → HCID 86705166、化合物

HRID 2401260ノート

反応式

HRID 2401260 の反応式
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]

参加物

5

反応物 3

HCID 11776TriphenylphosphineHCID 220568ethyl N-ethoxycarbonyliminocarbamateHCID 86705165HCID 86705165、化合物

生成物 1

HCID 86705166HCID 86705166、化合物収率 83.3%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-faaebe45a57142d3973c21322a5094c9
出典データセット
uspto-grants-2014_08
特許番号
US08796272B2

反応ノート

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