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Oxalyl chloride → HCID 68984731, 화합물

HRID 2249657
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HRID 2249657 반응식
[CH2:1]([N:6]1[C:10]2[CH:11]=[CH:12][C:13]([C:15](O)=[O:16])=[CH:14][C:9]=2[N:8]([CH2:18][CH2:19][CH:20]([CH3:22])[CH3:21])[C:7]1=[O:23])[CH2:2][CH:3]([CH3:5])[CH3:4].C(Cl)(=O)C(Cl)=O.[Cl-].[Al+3].[Cl-].[Cl-].[CH2:34]([O:39][C:40]1[CH:45]=[CH:44][CH:43]=[CH:42][C:41]=1[CH2:46][C:47]([O:49][CH2:50][CH2:51][CH:52]([CH3:54])[CH3:53])=[O:48])[CH2:35][CH:36]([CH3:38])[CH3:37]>C(Cl)Cl.CN(C)C=O>[CH2:1]([N:6]1[C:10]2[CH:11]=[CH:12][C:13]([C:15]([C:43]3[CH:44]=[CH:45][C:40]([O:39][CH2:34][CH2:35][CH:36]([CH3:38])[CH3:37])=[C:41]([CH2:46][C:47]([O:49][CH2:50][CH2:51][CH:52]([CH3:54])[CH3:53])=[O:48])[CH:42]=3)=[O:16])=[CH:14][C:9]=2[N:8]([CH2:18][CH2:19][CH:20]([CH3:22])[CH3:21])[C:7]1=[O:23])[CH2:2][CH:3]([CH3:5])[CH3:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 65578Oxalyl chlorideHCID 6451240Aluminum(III) ChlorideHCID 17816485HCID 17816485, 화합물HCID 17816487HCID 17816487, 화합물

생성물 1

HCID 68984731HCID 68984731, 화합물수율 91.6%

시약·촉매·용매 2

HCID 6228Dimethylformamide
용매
HCID 6344Dichloromethane용매2회

실험 절차

To a solution of 0.17 g of 1,3-diisopentyl-2-oxo-2,3-dihydro-1H-benzimidazole-5-carboxylic acid in 9 ml of methylene chloride are added 60 μl of oxalyl chloride and 20 μl of N,N-dimethylformamide successively. The mixture thus obtained is stirred at ambient temperature for 2 hours. Then, 0.42 g of aluminum chloride and 0.38 g of isopentyl 2-(2-isopentyloxyphenyl)acetate are successively added at ambient temperature, and the mixture thus obtained is stirred at the same temperature as above for 30 minutes. The reaction mixture is added to a mixture of methylene chloride and ice water, and the organic layer is separated. The organic layer thus obtained is washed with water and saturated aqueous solution of sodium chloride successively and dried over anhydrous magnesium sulfate, and the solvent is distilled off under reduced pressure. The residue is purified by silica gel column chromatography (eluent; hexane:ethyl acetate=5:1) to obtain 0.29 g of isopentyl 2-[5-[(1,3-diisopentyl-2-oxo-2,3-dihydro-1H-benzimidazol-5-yl)carbonyl]-2-(isopentyloxy)phenyl]acetate as a light yellow oily product.

후처리

  1. customThe mixture thus obtained
  2. customthe mixture thus obtained
  3. stirringis stirred at the same temperature as above for 30 minutes
  4. customthe organic layer is separated
  5. customThe organic layer thus obtained
  6. washis washed with water and saturated aqueous solution of sodium chloride successively
  7. dry with materialdried over anhydrous magnesium sulfate
  8. distillationthe solvent is distilled off under reduced pressure
  9. customThe residue is purified by silica gel column chromatography (eluent; hexane:ethyl acetate=5:1)

출처 및 근거

ORD 기록
ord-bb8cf0bef98145f7961495afb18dba85
출처 데이터셋
uspto-grants-2008_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07314888B1

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