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Chloromethyl Methyl Ether → HCID 131719456, 화합물

HRID 1734507
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HRID 1734507 반응식
[OH:1][CH2:2][C@@H:3]1[CH2:7][S:6][C:5]([S:8][CH3:9])=[N:4]1.[CH:10](N(C(C)C)CC)(C)C.Cl[CH2:20][O:21]C>ClCCl>[CH3:20][O:21][C@:3]1([CH2:2][O:1][CH3:10])[CH2:7][S:6][C:5]([S:8][CH3:9])=[N:4]1
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참가 물질

5

반응물 3

HCID 7864Chloromethyl Methyl EtherHCID 81531DiisopropylethylamineHCID 22862349(4R)-4,5-Dihydro-2-(methylthio)-4-thiazolemethanol

생성물 1

HCID 131719456HCID 131719456, 화합물수율 36%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

3.14 g of Compound (6) obtained in the step (a) and 6.7 ml of diisopropylethylamine were dissolved in 40 ml of dry dichloromethane solution. 2.33 g of chloromethylmethyl ether was added to the above mixture under ice-cooling and the reaction mixture was stirred for 1 hour under the same condition and for 15 hours at room temperature. After the reaction, the reaction mixture was washed with water, saturated sodium bicarbonate solution and saturated saline solution, and dried over magnesium sulfate. After removal of the solvent, the resulting residue was purified by silica gel column chromatography (chloroform-ethyl acetate) to give 1.42 g (36%) of 4(R)-methoxy-methyloxymethyl-2-methylthio-1,3-thiazoline [Compound (7)].

후처리

  1. temperaturecooling
  2. customAfter the reaction
  3. washthe reaction mixture was washed with water, saturated sodium bicarbonate solution and saturated saline solution
  4. dry with materialdried over magnesium sulfate
  5. customAfter removal of the solvent
  6. customthe resulting residue was purified by silica gel column chromatography (chloroform-ethyl acetate)

출처 및 근거

ORD 기록
ord-cdc12c897c9249a9b32294e176cb2c1d
출처 데이터셋
uspto-grants-1996_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05534510

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