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Ammonia → HCID 86711600, 화합물

HRID 527366
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HRID 527366 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].O>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

6

반응물 4

HCID 222AmmoniaHCID 962WaterHCID 24386Thionyl ChlorideHCID 580227444-(Cyclopropylsulfanyl)benzoic acid

생성물 1

HCID 86711600HCID 86711600, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Thionyl chloride (340 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 dichloromethane (1.9 mL), and the mixture is heated at reflux for 30 min. All volatiles are removed under reduced pressure, and the residue is dissolved in chloroform (1.9 mL). Concentrated aqueous ammonia (28%, 770 μL, 9.8 mmol) is added and the mixture is stirred at room temperature for 1 h. Water is added and the phases are separated. The organic layer is concentrated under reduced pressure. Yield: 137 mg (72% of theory); ESI mass spectrum: [M+H]+=194; r.t. HPLC: 0.45 min (X011_S03).

후처리

  1. temperaturethe mixture is heated
  2. temperatureat reflux for 30 min
  3. customAll volatiles are removed under reduced pressure
  4. dissolutionthe residue is dissolved in chloroform (1.9 mL)
  5. customthe phases are separated
  6. concentrationThe organic layer is concentrated under reduced pressure
  7. customr.t
  8. custom0.45 min (X011_S03)

출처 및 근거

ORD 기록
ord-3b6786a9f00d4aa2b3d057f4fe418bf7
출처 데이터셋
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09346794B1

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