O-(1,1-Dimethylethyl) S-(4,6-dimethyl-2-pyrimidinyl) carbonothioate → HCID 19960856、化合物

HRID 893854

反応式

HRID 893854 の反応式
C(OC([CH:6]1[CH:14]2[C:9]3([CH:18]=[CH:17][CH:16]=[CH:15][C:10]3=[N:11][CH2:12][CH2:13]2)[S:8][CH2:7]1)=O)C.[C:19]([O:23][C:24](SC1N=C(C)C=C(C)N=1)=[O:25])([CH3:22])([CH3:21])[CH3:20]>C(Cl)(Cl)Cl>[CH2:19]([O:23][C:24]([C:7]1([C:24]([O:23][C:19]([CH3:20])([CH3:21])[CH3:22])=[O:25])[S:8][C:9]23[CH:18]=[CH:17][CH:16]=[CH:15][C:10]2=[N:11][CH2:12][CH2:13][CH:14]3[CH2:6]1)=[O:25])[CH3:20]

参加物

4

反応物 2

HCID 148428O-(1,1-Dimethylethyl) S-(4,6-dimethyl-2-pyrimidinyl) carbonothioateHCID 19960928HCID 19960928、化合物

生成物 1

HCID 19960856HCID 19960856、化合物収率 123.3%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

In 20 ml of desiccated chloroform were dissolved 6 g of 1,2,3,4-tetrahydro-benzo[b]thieno[2,3-c]pyridinecarboxylic acid ethyl ester synthesized in Example 1 and 6.63 g of 2-(tertiary-butoxycarbonylthio)-4,6-dimethylpyrimidine, and the solution was refluxed for 30 minutes. After distilling off chloroform under reduced pressure, the residue was dissolved in 300 ml of ethyl acetate and the solution was washed thrice with 50 ml of an aqueous 5% sodium hydrogencarbonate, twice with an aqueous 5% citric acid solution, and then twice with a saturated aqueous sodium chloride solution and thereafter dried with sodium sulfate. Ethyl acetate was distilled off under reduced pressure and the residue was recrystallized from a mixture of chloroform and petroleum ether to provide 6.18 g (yield of 76%) of 2 -tert-butoxycarbonyl-1,2,3,4-tetrahydro-benzo[b]thieno[2,3-c]pyridine-carboxylic acid ethyl ester.

後処理

  1. temperaturethe solution was refluxed for 30 minutes
  2. distillationAfter distilling off chloroform under reduced pressure
  3. dissolutionthe residue was dissolved in 300 ml of ethyl acetate
  4. washthe solution was washed thrice with 50 ml of an aqueous 5% sodium hydrogencarbonate
  5. dry with materialtwice with an aqueous 5% citric acid solution, and then twice with a saturated aqueous sodium chloride solution and thereafter dried with sodium sulfate
  6. distillationEthyl acetate was distilled off under reduced pressure
  7. customthe residue was recrystallized from a mixture of chloroform and petroleum ether

出典と根拠

ORDレコード
ord-bbe968fc67424876a0b172b66841c7de
出典データセット
uspto-grants-1992_06
特許番号
US05126448

関連ノート

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