Chloride → HCID 25190241, 화합물

HRID 2410625노트

반응식

HRID 2410625 반응식
[CH2:1]([O:3][C:4](=[O:18])[CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][C:15](O)=[O:16])[CH3:2].[Cl-].O=S(Cl)Cl.Cl.[NH2:25][OH:26]>C(Cl)(Cl)Cl.ClCCl.N1C=CC=CC=1.C(OCC)(=O)C>[OH:26][NH:25][C:15](=[O:16])[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][C:4]([O:3][CH2:1][CH3:2])=[O:18]

참가 물질

9

반응물 4

HCID 312ChlorideHCID 24386Thionyl ChlorideHCID 443297Hydroxyamine hydrochlorideHCID 560435HCID 560435, 화합물

생성물 1

HCID 25190241HCID 25190241, 화합물수율 82%

시약·촉매·용매 4

HCID 1049Pyridine용매HCID 6212Chloroform용매HCID 6344Dichloromethane용매HCID 8857Ethyl Acetate용매

실험 절차

In a single-neck flask equipped with reflux condenser, under stirring and argon flux, the 12-ethoxy-12-oxododecanoic acid (13; 1.5 g, 5.8 mmol) is solved in chloroform (20 mL). Thionyle chloride is dropped (SOCl2; 0.64 mL, 8.8 mmol) and the reaction is carried on under reflux for 3 h. The mixture is cooled down to room temperature and the solvent is eliminated under high vacuum. The obtained product is solved in dichloromethane (20 mL) and is added, at room temperature and under stirring, with a solution of hydroxylamine hydrochloride (0.61 g, 8.8 mmol) in pyridine (10 mL) leaving to react for 12 h under the same conditions. All the solvent are eliminated under high vacuum and the remaining product is solubilised in ethyl acetate (50 mL), washed with distilled water (3×20 mL). The organic phase is anhydrified with anhydrous sodium sulphate and filtered under vacuum. The solvent is evaporated and dried under high vacuum to give 1.3 g (Yield=82%) of product as a pale yellow solid.

후처리

  1. customIn a single-neck flask equipped
  2. temperaturewith reflux condenser
  3. temperatureunder reflux for 3 h
  4. additionis added, at room temperature
  5. customleaving
  6. customto react for 12 h under the same conditions
  7. washwashed with distilled water (3×20 mL)
  8. filtrationfiltered under vacuum
  9. customThe solvent is evaporated
  10. customdried under high vacuum

출처 및 근거

ORD 기록
ord-dd5b592a288e439582a50d9f905114ae
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08816107B2

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