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Dimethylformamide → HCID 17816502、化合物

HRID 2249633
ノート
印刷プレビュー

反応式

HRID 2249633 の反応式
[CH2:1]([O:6][C:7]1[CH:8]=[C:9]([CH:13]=[CH:14][C:15]=1[O:16][CH2:17][CH2:18][CH:19]([CH3:21])[CH3:20])[C:10]([OH:12])=O)[CH2:2][CH:3]([CH3:5])[CH3:4].CN(C)C=O.[Cl-].[Al+3].[Cl-].[Cl-].[CH2:31]([O:36][C:37]1[CH:42]=[CH:41][CH:40]=[CH:39][C:38]=1[CH2:43][C:44]([O:46][CH2:47][CH2:48][CH:49]([CH3:51])[CH3:50])=[O:45])[CH2:32][CH:33]([CH3:35])[CH3:34]>C(Cl)Cl.C(Cl)(Cl)Cl>[CH2:1]([O:6][C:7]1[CH:8]=[C:9]([CH:13]=[CH:14][C:15]=1[O:16][CH2:17][CH2:18][CH:19]([CH3:21])[CH3:20])[C:10]([C:40]1[CH:41]=[CH:42][C:37]([O:36][CH2:31][CH2:32][CH:33]([CH3:35])[CH3:34])=[C:38]([CH2:43][C:44]([O:46][CH2:47][CH2:48][CH:49]([CH3:50])[CH3:51])=[O:45])[CH:39]=1)=[O:12])[CH2:2][CH:3]([CH3:4])[CH3:5]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 6228DimethylformamideHCID 6451240Aluminum(III) ChlorideHCID 17816448HCID 17816448、化合物HCID 17816487HCID 17816487、化合物

生成物 1

HCID 17816502HCID 17816502、化合物収率 77.6%

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒
HCID 6344
Dichloromethane
溶媒

実験手順

In 8 ml of methylene chloride is dissolved 0.80 g of 3,4-diisopentyloxybenzoic acid. Then, 20 μl of N,N-dimethylformamide is added, and the mixture thus obtained is stirred at ambient temperature for one hour. To the mixture thus obtained are successively added 1.10 g of aluminum chloride and 0.95 g of isopentyl 2-(2-isopentyloxyphenyl)acetate at 5-10° C., and the mixture thus obtained is stirred at 5-10° C. for 10 minutes. The reaction mixture is added to a mixture of chloroform and ice water, and the organic layer is separated. After washing the organic layer with water and saturated aqueous solution of sodium chloride successively and dried over anhydrous magnesium sulfate, the solvent is distilled off under reduced pressure. The residue thus obtained is purified by silica gel column chromatography [eluent; hexane:ethyl acetate=10:1] to obtain 1.20 g of isopentyl 2-[5-(3,4-diisopentyloxybenzoyl)-2-isopentyloxyphenyl]-acetate as a yellow oily product.

後処理

  1. customthe mixture thus obtained
  2. customTo the mixture thus obtained
  3. customat 5-10° C.
  4. customthe mixture thus obtained
  5. stirringis stirred at 5-10° C. for 10 minutes
  6. customthe organic layer is separated
  7. washAfter washing the organic layer with water and saturated aqueous solution of sodium chloride successively
  8. dry with materialdried over anhydrous magnesium sulfate
  9. distillationthe solvent is distilled off under reduced pressure
  10. customThe residue thus obtained
  11. customis purified by silica gel column chromatography [eluent; hexane:ethyl acetate=10:1]

出典と根拠

ORDレコード
ord-44d9de3cf8c844979a84a13546446f09
出典データセット
uspto-grants-2008_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07314888B1

反応ノート

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