Hydrochloric Acid → HCID 22063454, 화합물

HRID 12097노트

반응식

HRID 12097 반응식
[CH2:1]([C:3]1[CH:8]=[CH:7][C:6]([CH2:9][C:10]([NH:13]C(=O)C)([CH3:12])[CH3:11])=[CH:5][CH:4]=1)[CH3:2].[OH-].[K+].Cl.C(OCC)C>C(O)CO.C(#N)C>[CH2:1]([C:3]1[CH:8]=[CH:7][C:6]([CH2:9][C:10]([NH2:13])([CH3:12])[CH3:11])=[CH:5][CH:4]=1)[CH3:2]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 14797Potassium HydroxideHCID 22063473HCID 22063473, 화합물

생성물 1

HCID 22063454HCID 22063454, 화합물

시약·촉매·용매 2

HCID 174Ethylene Glycol용매HCID 6342Acetonitrile용매

실험 절차

16.3 g (74 mmol) of N-[2-(4-ethylphenyl)-1,1-dimethylethyl]acetamide and 8.0 g of potassium hydroxide are refluxed for 15 hours in 60 mL ethylene glycol. The reaction mixture is combined with ice water and extracted three times with diethyl ether. The combined organic phases are washed with water, dried with sodium sulfate, and freed from solvent. To prepare the hydrochloride, the crude product is dissolved in acetonitrile and ethereal hydrochloric acid and diethyl ether are added successively. The solid precipitated is suction filtered and dried. Yield: 11.0 g (69%, hydrochloride); melting point 165° C.-167° C.

후처리

  1. extractionextracted three times with diethyl ether
  2. washThe combined organic phases are washed with water
  3. dry with materialdried with sodium sulfate
  4. customTo prepare the hydrochloride
  5. customThe solid precipitated
  6. filtrationfiltered
  7. customdried

출처 및 근거

ORD 기록
ord-d40536500a4f4ac6b14cb0966f32001e
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07727984B2

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