Triethylamine → 4,8-Dichloro-5-methyl-6-ethoxycarbonylthiochroman

HRID 1275461노트

반응식

HRID 1275461 반응식
O[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.C(N(CC)CC)C.CS([Cl:30])(=O)=O>C(Cl)Cl>[Cl:30][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

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 234506678-Chloro-6-ethoxycarbonyl-5-methylthiochroman-4-ol

생성물 1

HCID 221183894,8-Dichloro-5-methyl-6-ethoxycarbonylthiochroman수율 116.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

1.0 Gram (3.5 mmol) of 4-hydroxy-5-methyl-6-ethoxycarbonyl-8-chlorothiochroman was dissolved in 5 ml of methylene chloride, and 0.72 ml (5.2 mmol) of triethylamine and 0.4 ml (5.2 mmol) of methanesulfonyl chloride were added with an ice bath cooling. The mixture was stirred at room temperature for 1 hour. After the completion of the reaction, an organic layer was washed with 2N hydrochloric acid and with a saturated sodium hydrogencarbonate aqueous solution and dried over anhydrous sodium sulfate, and the solvent was distilled off to give 1.24 g (yield 100%) of 4,8-dichloro-5-methyl-6-ethoxycarbonylthiochroman.

후처리

  1. temperaturecooling
  2. customAfter the completion of the reaction
  3. washan organic layer was washed with 2N hydrochloric acid and with a saturated sodium hydrogencarbonate aqueous solution
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationthe solvent was distilled off

출처 및 근거

ORD 기록
ord-f78baf194a5f43f8a5b957b850dcd66e
출처 데이터셋
uspto-grants-2000_12
특허 번호
US06159904

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