Triphenylphosphine → HCID 68565032、化合物

HRID 1593546ノート

反応式

HRID 1593546 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[OH:12])[O:8][C:7]([CH3:14])([CH3:13])[CH:6]=[C:5]2[C:15]([F:18])([F:17])[F:16].O[CH2:20][CH2:21][CH2:22][O:23][C:24]1[CH:38]=[CH:37][C:27]([O:28][C:29]([CH3:36])([CH2:34][CH3:35])[C:30]([O:32][CH3:33])=[O:31])=[CH:26][CH:25]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.N(C(OCC)=O)=NC(OCC)=O>C1COCC1>[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[O:12][CH2:20][CH2:21][CH2:22][O:23][C:24]1[CH:38]=[CH:37][C:27]([O:28][C:29]([CH3:36])([CH2:34][CH3:35])[C:30]([O:32][CH3:33])=[O:31])=[CH:26][CH:25]=1)[O:8][C:7]([CH3:14])([CH3:13])[CH:6]=[C:5]2[C:15]([F:16])([F:18])[F:17]

参加物

6

反応物 4

HCID 11776TriphenylphosphineHCID 220568ethyl N-ethoxycarbonyliminocarbamateHCID 665248776-Chloro-2,2-dimethyl-4-(trifluoromethyl)-2H-chromen-7-olHCID 68565476HCID 68565476、化合物

生成物 1

HCID 68565032HCID 68565032、化合物収率 61.8%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 6-Chloro-2,2-dimethyl-4-(trifluoromethyl)-2H-chromen-7-ol (0.66 g, 2.95 mmol), methyl 2-(4-(3-hydroxypropoxy)phenoxy)-2-methylbutanoate (1.0 g, 2.97 mmol) and triphenylphosphine (0.85 g, 3.24 mmol) in 25 mL THF is added diethyl azodicarboxylate (0.56 g, 3.21 mmol)(slight exotherm) and the reaction mixture is stirred at ambient temperature overnight (16 h). After concentrating under reduced pressure, the residue obtained is chromatographed over silica gel to provide methyl 2-(4-(3-((6-chloro-2,2-dimethyl-4-(trifluoromethyl)-2H-chromen-7-yl)oxy)propoxy)phenoxy)-2-methylbutanoate (0.99 g).

後処理

  1. concentrationAfter concentrating under reduced pressure
  2. customthe residue obtained
  3. customis chromatographed over silica gel

出典と根拠

ORDレコード
ord-5d26e891d5f04f90b4e53f5c1d4be094
出典データセット
uspto-grants-2007_11
特許番号
US07297715B2

反応ノート

読み込み中…