Triethylamine → 3-Oxo-3-(2-phenyl-1,3-dioxan-5-yloxy)propyl 2-propylpentanoate

HRID 41815

反応式

HRID 41815 の反応式
[CH2:1]([CH:4]([CH2:13][CH2:14][CH3:15])[C:5]([O:7][CH2:8][CH2:9][C:10]([OH:12])=[O:11])=[O:6])[CH2:2][CH3:3].[CH2:16]1[O:21][CH:20]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[O:19][CH2:18][CH:17]1O.C(N(CC)CC)C>C(Cl)Cl>[CH2:13]([CH:4]([CH2:1][CH2:2][CH3:3])[C:5]([O:7][CH2:8][CH2:9][C:10](=[O:12])[O:11][CH:17]1[CH2:18][O:19][CH:20]([C:22]2[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=2)[O:21][CH2:16]1)=[O:6])[CH2:14][CH3:15]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 743621,3-Dioxan-5-ol, 2-phenyl-HCID 584552543-(2-Propylpentanoyloxy)propanoic acid

生成物 1

HCID 584552943-Oxo-3-(2-phenyl-1,3-dioxan-5-yloxy)propyl 2-propylpentanoate収率 83%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

3-(2-propylpentanoyloxy)propanoic acid (2.05 g, 9.5 mmol) was dissolved in anhydrous CH2Cl2 (200 ml) under argon. 1,3-O-benzylideneglycerol (2.50 g, 13.67 mmol triethylamine (4.04 g, 40.0 mmol) and O-benzotriazol-1-yl-N,N, N′,N′-trimethyluronium hexafluorophosphate (4.2 g, 11.0 mmol) were added successively. The reaction mixture was stirred under argon for 72 h. The reaction mixture was washed with saturated NaHCO3 solution (1×90 ml), water (1×90 ml) and dried over Na2SO4. The organic solvent was removed under reduced pressure giving a pale, pink solid (2.99 g, 7.9 mmol, 83%).

後処理

  1. washThe reaction mixture was washed with saturated NaHCO3 solution (1×90 ml), water (1×90 ml)
  2. dry with materialdried over Na2SO4
  3. customThe organic solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-4a51801403a442a797ece5a653e5e9ec
出典データセット
uspto-grants-2013_09
特許番号
US08535655B2

関連ノート

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