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Hydroxy-(hydroxy(dioxo)chromio)oxy-dioxochromium;pyridine → HCID 57097671, 화합물

HRID 2211329
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HRID 2211329 반응식
[CH3:1][C@@:2]12[CH2:8][CH:5]([CH2:6][CH2:7]1)[CH2:4][CH:3]2[OH:9].[Cr](O[Cr](O)(=O)=O)(O)(=O)=O.N1C=CC=CC=1>C(Cl)Cl.C(OCC)C>[CH3:1][C@@:2]12[CH2:8][CH:5]([CH2:6][CH2:7]1)[CH2:4][C:3]2=[O:9]
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참가 물질

5

반응물 2

HCID 18757208Hydroxy-(hydroxy(dioxo)chromio)oxy-dioxochromium;pyridineHCID 57313420HCID 57313420, 화합물

생성물 1

HCID 57097671HCID 57097671, 화합물수율 64.5%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 6344Dichloromethane용매2회

실험 절차

79.6 g (0.63M) of the optically active alcohol (V) obtained in 1-4) above was dissolved in 300 ml of methylene chloride and the resulting solution was added dropwise to a suspension of 304 g (0.81M) of pyridine dichromate in 700 ml of methylene chloride at room temperature. Then the resulting mixture was stirred for three days. The obtained reaction mixture was diluted with 1 l of diethyl ether and filtered through celite. The filtrate was dried over anhydrous magnesium sulfate and the solvent was evaporated. The residue was distilled under reduced pressure to give 50.4 g (theoretical yield: 64.5%) of the aimed compound (VI) as a colorless oily material. b.p.: 70° C./20 mmHg.

후처리

  1. customThe obtained reaction mixture
  2. filtrationfiltered through celite
  3. dry with materialThe filtrate was dried over anhydrous magnesium sulfate
  4. customthe solvent was evaporated
  5. distillationThe residue was distilled under reduced pressure

출처 및 근거

ORD 기록
ord-08c384a4b6ec466aa3f88e5e2a55a50b
출처 데이터셋
uspto-grants-1995_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05463118

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