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Methane, dichloromethoxy- → HCID 15516676, 화합물

HRID 323803
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HRID 323803 반응식
[C:1]([NH:4][C:5]([CH2:16][CH2:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)([CH2:11][O:12][C:13](=[O:15])[CH3:14])[CH2:6][O:7][C:8](=[O:10])[CH3:9])(=[O:3])[CH3:2].[CH3:24][O:25]C(Cl)Cl>ClCCl.[Ti](Cl)(Cl)(Cl)Cl>[C:1]([NH:4][C:5]([CH2:16][CH2:17][C:18]1[CH:23]=[CH:22][C:21]([CH:24]=[O:25])=[CH:20][CH:19]=1)([CH2:11][O:12][C:13](=[O:15])[CH3:14])[CH2:6][O:7][C:8](=[O:10])[CH3:9])(=[O:3])[CH3:2]
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참가 물질

5

반응물 2

HCID 21004Methane, dichloromethoxy-HCID 10543752Acetamide, N-[1,1-bis[(acetyloxy)methyl]-3-phenylpropyl]-

생성물 1

HCID 15516676HCID 15516676, 화합물

시약·촉매·용매 2

HCID 24193Titanium Tetrachloride촉매HCID 6344Dichloromethane용매

실험 절차

To a solution of 2-acetamido-1, 3-diacetoxy-2-(2-phenylethyl)propane (10 g) in anhydrous dichloromethane (150 ml) were added titanium tetrachloride (15.4 ml) and dichloromethyl methyl ether (5.63 ml) under a nitrogen atmosphere at −15° C. The mixture was stirred at room temperature for 2 hours, poured into ice water and extracted with chloroform. The chloroform layer was washed with water, a saturated aqueous sodium hydrogencarbonate solution and saturated brine, dried over anhydrous magnesium sulfate and the solvent was distilled away under reduced pressure. The obtained residue was purified by silica gel column chromatography (eluent; diisopropyl ether: ethyl acetate =1:1) to give the title compound (5.1 g) as a white solid, melting point 98-100° C.

후처리

  1. extractionextracted with chloroform
  2. washThe chloroform layer was washed with water
  3. dry with materiala saturated aqueous sodium hydrogencarbonate solution and saturated brine, dried over anhydrous magnesium sulfate
  4. distillationthe solvent was distilled away under reduced pressure
  5. customThe obtained residue was purified by silica gel column chromatography (eluent; diisopropyl ether: ethyl acetate =1:1)

출처 및 근거

ORD 기록
ord-628b0ac45bfb44b6a60b13cb6e5ca068
출처 데이터셋
uspto-grants-2001_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06214873B1

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