Triphenylphosphine → HCID 59536867、化合物

HRID 220655ノート

反応式

HRID 220655 の反応式
[CH3:1][S:2]([CH2:4][CH:5]([NH:16][C:17](=[O:23])[O:18][C:19]([CH3:22])([CH3:21])[CH3:20])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[C:12]([F:15])([F:14])[F:13])=O.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>ClC(Cl)(Cl)Cl>[CH3:1][S:2][CH2:4][CH:5]([NH:16][C:17](=[O:23])[O:18][C:19]([CH3:21])([CH3:20])[CH3:22])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[C:12]([F:15])([F:14])[F:13]

参加物

4

反応物 2

HCID 11776TriphenylphosphineHCID 59536884tert-Butyl {2-(methylsulphinyl)-1-[2-(trifluoromethyl)phenyl]ethyl}carbamate

生成物 1

HCID 59536867HCID 59536867、化合物

試薬・触媒・溶媒 1

HCID 5943Carbon Tetrachloride溶媒

実験手順

Of the compound from Example 108A, 400 mg (1.14 mmol), and 567 mg (2.16 mmol) of triphenylphosphine, were dissolved in 14 ml of tetrachloromethane. The reaction mixture was stirred overnight at reflux temperature and then freed from the solvent on a rotary evaporator. The residue was purified by preparative HPLC [Method 20]. The product fraction was freed from the solvent on a rotary evaporator. Drying in an HV gave 340 mg (85% of theory) of the title compound.

後処理

  1. temperatureat reflux temperature
  2. customfreed from the solvent on a rotary evaporator
  3. customThe residue was purified by preparative HPLC [Method 20]
  4. customThe product fraction was freed from the solvent on a rotary evaporator
  5. customDrying in an HV

出典と根拠

ORDレコード
ord-ebc22034d37a443891cb3c1d656fcdac
出典データセット
uspto-grants-2012_06
特許番号
US08202895B2

反応ノート

読み込み中…