Triphenylphosphine → HCID 86604655、化合物

HRID 1593548ノート

反応式

HRID 1593548 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[O:12][CH2:13][CH2:14][CH2:15][OH:16])[O:8][C:7]([CH3:18])([CH3:17])[CH:6]=[C:5]2[C:19]([F:22])([F:21])[F:20].O[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][CH2:13][CH2:14][CH2:15][O:16][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]([CH3:18])([CH3:17])[CH:6]=[C:5]2[C:19]([F:20])([F:22])[F:21]

参加物

6

反応物 4

HCID 11776TriphenylphosphineHCID 220568ethyl N-ethoxycarbonyliminocarbamateHCID 11996320(2S)-Methyl 2-(4-hydroxyphenoxy)-2-methylbutanoateHCID 68565082HCID 68565082、化合物

生成物 1

HCID 86604655HCID 86604655、化合物収率 61%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 3-((6-chloro-2,2-dimethyl-4-(trifluoromethyl)-2H-chromen-7-yl)oxy)propan-1-ol (0.5 g, 1.48 mmol), (2S)-Methyl 2-(4-hydroxyphenoxy)-2-methylbutanoate (0.35 g, 1.56 mmol), and triphenylphosphine (0.42 g, 1.6 mmol) in THF (20 mL) was added diethyl azodicarboxylate (0.28 g, 1.6 mmol) and the solution stirred at ambient temperature for 16 h. After concentrating under reduced pressure, the residue thus obtained was chromatographed over silica gel using AcOEt/hexanes to furnish the desired compound (0.49 g).

後処理

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

出典と根拠

ORDレコード
ord-a10bcdb3089840468c2930b41e0f2cb3
出典データセット
uspto-grants-2007_11
特許番号
US07297715B2

反応ノート

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