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Water → 4-Ethylthio-5-methyl-6-ethoxycarbonyl-8-chlorothiochroman

HRID 1275462
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HRID 1275462 반응식
Cl[CH:2]1[C:11]2[C:6](=[C:7]([Cl:18])[CH:8]=[C:9]([C:13]([O:15][CH2:16][CH3:17])=[O:14])[C:10]=2[CH3:12])[S:5][CH2:4][CH2:3]1.[CH2:19]([SH:21])[CH3:20].C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[CH2:19]([S:21][CH:2]1[C:11]2[C:6](=[C:7]([Cl:18])[CH:8]=[C:9]([C:13]([O:15][CH2:16][CH3:17])=[O:14])[C:10]=2[CH3:12])[S:5][CH2:4][CH2:3]1)[CH3:20]
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참가 물질

6

반응물 4

HCID 962WaterHCID 6343EthanethiolHCID 11430Potassium CarbonateHCID 221183894,8-Dichloro-5-methyl-6-ethoxycarbonylthiochroman

생성물 1

HCID 221184604-Ethylthio-5-methyl-6-ethoxycarbonyl-8-chlorothiochroman수율 139.5%

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

실험 절차

0.8 Gram (2.6 mmol) of 4,8-dichloro-5-methyl-6-ethoxycarbonylthiochroman was dissolved in 5 ml of N,N-dimethylformamide, and 0.15 ml (3.1 mmol) of ethanethiol and 0.43 g (3.1 mmol) of potassium carbonate were added. The mixture was stirred at room temperature for 2 days. After the completion of the reaction, 20 ml of water was added, and the reaction mixture was extracted with ethyl acetate twice. An organic layer was washed with water and with a saturated sodium chloride aqueous solution and dried over anhydrous sodium sulfate, and the solvent was distilled off to give 1.2 g (yield 100%) of 4-ethylthio-5-methyl-6-ethoxycarbonyl-8-chlorothiochroman.

후처리

  1. additionwas added
  2. extractionthe reaction mixture was extracted with ethyl acetate twice
  3. washAn organic layer was washed with water and with a saturated sodium chloride aqueous solution
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationthe solvent was distilled off

출처 및 근거

ORD 기록
ord-45552dfeec094c4b80d0b9b39424fe67
출처 데이터셋
uspto-grants-2000_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06159904

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