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Ammonia → HCID 86711600, 화합물

HRID 524347
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HRID 524347 반응식
S(Cl)(Cl)=O.[CH:5]1([S:8][C:9]2[CH:17]=[CH:16][C:12]([C:13](O)=[O:14])=[CH:11][CH:10]=2)[CH2:7][CH2:6]1.[NH3:18]>ClCCl>[CH:5]1([S:8][C:9]2[CH:17]=[CH:16][C:12]([C:13]([NH2:18])=[O:14])=[CH:11][CH:10]=2)[CH2:7][CH2:6]1
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참가 물질

5

반응물 3

HCID 222AmmoniaHCID 24386Thionyl ChlorideHCID 580227444-(Cyclopropylsulfanyl)benzoic acid

생성물 1

HCID 86711600HCID 86711600, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Thionylchloride (342 μL, 4.7 mmol) is added to a solution of 4-cyclopropylsulfanyl-benzoic acid (prepared as described in WO07003960, 190 mg, 0.98 mmol) in dichloro-methane (1.9 mL). The mixture is heated at reflux for 30 min and concentrated under reduced pressure. The residue is treated with toluene, and all volatiles are evaporated. The residue is dissolved in chloroform (1.9 mL) and treated with concentrated aqueous ammonia (770 μL, 9.8 mmol). The mixture is stirred at room temperature for 1 h and then extracted with water. The organic layer is dried over Na2SO4 and concentrated under reduced pressure. Yield: 137 mg (72% of theory); ESI mass spectrum: [M+H]+=194; Retention time HPLC: 0.45 min (X011_S03).

후처리

  1. temperatureThe mixture is heated
  2. temperatureat reflux for 30 min
  3. concentrationconcentrated under reduced pressure
  4. additionThe residue is treated with toluene
  5. customall volatiles are evaporated
  6. dissolutionThe residue is dissolved in chloroform (1.9 mL)
  7. extractionextracted with water
  8. dry with materialThe organic layer is dried over Na2SO4
  9. concentrationconcentrated under reduced pressure
  10. custom0.45 min (X011_S03)

출처 및 근거

ORD 기록
ord-ac918964e5eb48abb0f8e35f6aae8456
출처 데이터셋
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09340507B2

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