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Methanethiol → HCID 3642305, 화합물

HRID 1733649
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HRID 1733649 반응식
CS[C:3]([C:9]1[CH:14]=[CH:13][C:12]([C:15]([C:17]2[S:18][CH:19]=[CH:20][CH:21]=2)=[O:16])=[CH:11][CH:10]=1)([CH3:8])[C:4]([O:6][CH3:7])=[O:5].[Na].CS.[Cl-].[NH4+]>CO>[S:18]1[CH:19]=[CH:20][CH:21]=[C:17]1[C:15]([C:12]1[CH:13]=[CH:14][C:9]([CH:3]([CH3:8])[C:4]([O:6][CH3:7])=[O:5])=[CH:10][CH:11]=1)=[O:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 878MethanethiolHCID 25517Ammonium ChlorideHCID 5360545SodiumHCID 12917659HCID 12917659, 화합물

생성물 1

HCID 3642305HCID 3642305, 화합물수율 47.5%

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

Methyl α-methylthio-α-[p-(2-thienylcarbonyl)-phenyl]propionate (288 mg) was dissolved in 1 ml of anhydrous methanol, and 1.0 ml of a methanol solution (2.34 M) of sodium salt of methyl mercaptan was added. The mixture was stirred at room temperature for 1 hour and heated under reflux for 30 minutes. After cooling, an aqueous solution of ammonium chloride (1.5 g/20 ml) was added to the reaction mixture. The mixture was extracted with 20 ml of methylene chloride and twice with 10 ml of methylene chloride. The extract was washed with 20 ml of a saturated aqueous solution of sodium hydrogen carbonate and with 10 ml of water, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to afford 117 mg of methyl α-[p-(2-thienylcarbonyl)phenyl]propionate in a yield of 47%.

후처리

  1. temperatureheated
  2. temperatureunder reflux for 30 minutes
  3. temperatureAfter cooling
  4. extractionThe mixture was extracted with 20 ml of methylene chloride and twice with 10 ml of methylene chloride
  5. washThe extract was washed with 20 ml of a saturated aqueous solution of sodium hydrogen carbonate and with 10 ml of water
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-68a9fabe328349fc8cdb451347ba69de
출처 데이터셋
uspto-grants-1980_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04242519

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