Triethylamine → HCID 54343021、化合物

HRID 1872397

反応式

HRID 1872397 の反応式
[C:1]([C:4]1[CH:14]=[CH:13][C:7]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[CH:6][CH:5]=1)(=[O:3])[CH3:2].[CH2:15]([O:20][C:21]1[CH:28]=[CH:27][C:24]([CH:25]=O)=[CH:23][CH:22]=1)[CH2:16][CH2:17][CH2:18][CH3:19].C(N(CC)CC)C>ClCCl.C(OCC)(=O)C.[Ti](Cl)(Cl)(Cl)Cl>[CH2:15]([O:20][C:21]1[CH:28]=[CH:27][C:24]([CH:25]=[CH:2][C:1]([C:4]2[CH:14]=[CH:13][C:7]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[CH:6][CH:5]=2)=[O:3])=[CH:23][CH:22]=1)[CH2:16][CH2:17][CH2:18][CH3:19]

参加物

7

反応物 3

HCID 8471TriethylamineHCID 79815p-PentoxybenzaldehydeHCID 600911Ethyl 4-acetylbenzoate

生成物 1

HCID 54343021HCID 54343021、化合物収率 61.2%

試薬・触媒・溶媒 3

HCID 24193Titanium Tetrachloride触媒HCID 6344Dichloromethane溶媒3 回HCID 8857Ethyl Acetate溶媒

反応条件

温度
0 °C

実験手順

To a solution of titanium(IV) chloride (13.88 g) in dichloromethane (100 ml) was added Ethyl 4-acetylbenzoate (11.53 g) and 4-n-pentyloxybenzaldehyde (12.68 g) in dichloromethane (50 ml) was added dropwise at 0° C. To the mixture was added triethylamine (12.44 ml) in dichloromethane (30 ml). The mixture was stirred at 0° C. for 30 minutes and diluted with ethyl acetate. The organic layer was washed with water (four times) and brine and dried over magnesium sulfate. The solvents were removed under reduced pressure and the residue was triturated with n-hexane. The solid was collected by filtration and dried to give 1-(4-n-Pentyloxyphenyl)-3-(4-ethoxycarbonylphenyl)-1-propen-3-one (13.45 g).

後処理

  1. additionwas added dropwise at 0° C
  2. washThe organic layer was washed with water (four times) and brine
  3. dry with materialdried over magnesium sulfate
  4. customThe solvents were removed under reduced pressure
  5. customthe residue was triturated with n-hexane
  6. filtrationThe solid was collected by filtration
  7. customdried

出典と根拠

ORDレコード
ord-5929b187f2df40f981646c2892dd1128
出典データセット
uspto-grants-2000_08
特許番号
US06107458

関連ノート

読み込み中…