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

HRID 1275461ノート

反応式

HRID 1275461 の反応式
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

参加物

5

反応物 3

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

生成物 1

HCID 221183894,8-Dichloro-5-methyl-6-ethoxycarbonylthiochroman収率 116.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f78baf194a5f43f8a5b957b850dcd66e
出典データセット
uspto-grants-2000_12
特許番号
US06159904

反応ノート

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