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Formic Acid → HCID 17816453, 화합물

HRID 2249698
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HRID 2249698 반응식
Br[C:2]1[C:10]2[N:9]([CH2:11][CH2:12][CH:13]([CH3:15])[CH3:14])[C:8](=[O:16])[N:7]([CH2:17][CH2:18][CH:19]([CH3:21])[CH3:20])[C:6]=2[CH:5]=[C:4](Br)[C:3]=1[C:23]([O:25][CH3:26])=[O:24].C(O)=O.C(N(CC)CC)C.Cl>CN(C)C=O.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.O.C(OCC)(=O)C>[CH2:17]([N:7]1[C:6]2[CH:5]=[CH:4][C:3]([C:23]([O:25][CH3:26])=[O:24])=[CH:2][C:10]=2[N:9]([CH2:11][CH2:12][CH:13]([CH3:15])[CH3:14])[C:8]1=[O:16])[CH2:18][CH:19]([CH3:21])[CH3:20]
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참가 물질

9

반응물 4

HCID 284Formic AcidHCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 17816478HCID 17816478, 화합물

생성물 1

HCID 17816453HCID 17816453, 화합물수율 77.9%

시약·촉매·용매 4

HCID 178418397HCID 178418397, 화합물
촉매
HCID 962Water용매
HCID 6228Dimethylformamide용매
HCID 8857Ethyl Acetate용매

반응 조건

온도
100 °C

실험 절차

In 7 ml of N,N-dimethylformamide are suspended 0.70 g of methyl 4,6-dibromo-1,3-diisopentyl-2-oxo-2,3-dihydro-1H-benzimidazole-5-carboxylate, 0.16 g of tetrakis(triphenylphosphine)palladium(0), 0.44 ml of formic acid and 2.4 ml of triethylamine. The suspension is stirred at 100° C. for 3 hours. The reaction mixture is added to a mixture of ethyl acetate and water, pH is adjusted to 4 with 2 mol/L hydrochloric acid, 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 then the solvent is distilled off under reduced pressure. The residue thus obtained is purified by silica gel column chromatography (eluent; hexane:ethyl acetate=5:1) to obtain 0.37 g of methyl 1,3-diisopentyl-2-oxo-2,3-dihydro-1H-benzimidazole-5-carboxylate as a colorless oily product.

후처리

  1. customthe organic layer is separated
  2. customThe organic layer thus obtained
  3. washis washed with water and saturated aqueous solution of sodium chloride successively
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationthe solvent is distilled off under reduced pressure
  6. customThe residue thus obtained
  7. customis purified by silica gel column chromatography (eluent; hexane:ethyl acetate=5:1)

출처 및 근거

ORD 기록
ord-74901506a3a0406d9f6e947b3bde71a6
출처 데이터셋
uspto-grants-2008_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07314888B1

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