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Dimethylformamide → HCID 17816502, 화합물

HRID 2249633
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HRID 2249633 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 6228DimethylformamideHCID 6451240Aluminum(III) ChlorideHCID 17816448HCID 17816448, 화합물HCID 17816487HCID 17816487, 화합물

생성물 1

HCID 17816502HCID 17816502, 화합물수율 77.6%

시약·촉매·용매 2

HCID 6212Chloroform용매
HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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]

출처 및 근거

ORD 기록
ord-44d9de3cf8c844979a84a13546446f09
출처 데이터셋
uspto-grants-2008_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07314888B1

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