Dichloromethane → 2-(2-methoxyphenethyl)imino-N-(ethylthiocarbamoyl)-5,5-dimethyl-1,3-thiazine

HRID 350637노트

반응식

HRID 350637 반응식
[CH3:1][O:2][C:3]1[CH:19]=[CH:18][CH:17]=[CH:16][C:4]=1[CH2:5][CH2:6][N:7]=[C:8]1[N:13]=[CH:12][C:11]([CH3:15])([CH3:14])[CH2:10][S:9]1.[CH2:20]([N:22]([CH2:25]C)CC)[CH3:21].ClCCl.C(Cl)(=[S:34])OCC>O>[CH3:1][O:2][C:3]1[CH:19]=[CH:18][CH:17]=[CH:16][C:4]=1[CH2:5][CH2:6][N:7]=[C:8]1[N:13]([C:25](=[S:34])[NH:22][CH2:20][CH3:21])[CH2:12][C:11]([CH3:15])([CH3:14])[CH2:10][S:9]1

참가 물질

6

반응물 4

HCID 6344DichloromethaneHCID 8471TriethylamineHCID 5325481O-ethyl chloromethanethioateHCID 226399872-(2-Methoxyphenethyl)imino-5,5-dimethyl-1,3-thiazine

생성물 1

HCID 226399822-(2-methoxyphenethyl)imino-N-(ethylthiocarbamoyl)-5,5-dimethyl-1,3-thiazine수율 60%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a mixture of 2-(2-methoxyphenethyl)imino-5,5-dimethyl-1,3-thiazine (0.28 g), triethylamine (0.15 g) and dichloromethane (5 ml) was added dropwise for 3 minutes ethyl chlorothiocarbonate (0.15 g). The mixture was stirred at room temperature for 2 hours. To the solution was added water (30 ml). The mixture was extracted with diethylether (60 ml), dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (n-hexane/ethyl acetate) to give 2-(2-methoxyphenethyl)imino-N-(ethylthiocarbamoyl)-5,5-dimethyl-1,3-thiazine (0.21 g, yield: 60%) as colorless oil.

후처리

  1. extractionThe mixture was extracted with diethylether (60 ml)
  2. dry with materialdried over anhydrous magnesium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customThe obtained residue was purified by silica gel column chromatography (n-hexane/ethyl acetate)

출처 및 근거

ORD 기록
ord-7a469e139c884c078235231610693182
출처 데이터셋
uspto-grants-2007_02
특허 번호
US07183275B2

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