4-Iodomethyl-tetrahydro-pyran-4-carboxylic acid methyl ester → Methyl 4-[(acetylsulfanyl)methyl]oxane-4-carboxylate

HRID 992422

반응식

HRID 992422 반응식
[CH3:1][O:2][C:3]([C:5]1([CH2:11]I)[CH2:10][CH2:9][O:8][CH2:7][CH2:6]1)=[O:4].[C:13]([O-:16])(=[S:15])[CH3:14].[K+]>CN(C)C=O.O>[CH3:1][O:2][C:3]([C:5]1([CH2:11][S:15][C:13](=[O:16])[CH3:14])[CH2:10][CH2:9][O:8][CH2:7][CH2:6]1)=[O:4]

참가 물질

5

반응물 2

HCID 227197884-Iodomethyl-tetrahydro-pyran-4-carboxylic acid methyl esterHCID 23670855Potassium ethanethioate

생성물 1

HCID 23448262Methyl 4-[(acetylsulfanyl)methyl]oxane-4-carboxylate수율 97%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

4-Iodomethyl-tetrahydro-pyran-4-carboxylic acid methyl ester (3.05 g) was dissolved in N,N-dimethylformamide (20 ml) at room temperature and potassium thioacetate (1.47 g) added. The mixture was stirred for 18 hours then diluted with water (50 ml) and extracted with diethyl ether (4×25 ml). The combined organics were washed with saturated sodium bicarbonate solution (3×20 ml) and brine (20 ml), then dried (MgSO4), filtered and evaporated under reduced pressure to give the title compound as a yellow solid (2.42 g, 97%).

후처리

  1. extractionextracted with diethyl ether (4×25 ml)
  2. washThe combined organics were washed with saturated sodium bicarbonate solution (3×20 ml) and brine (20 ml)
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-f01756040371460aaa3fd9d5afcad193
출처 데이터셋
uspto-grants-2002_10
특허 번호
US06469020B2

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