Hydrochloric Acid → HCID 22063454、化合物

HRID 1827752ノート

反応式

HRID 1827752 の反応式
[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]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 14797Potassium HydroxideHCID 22063473HCID 22063473、化合物

生成物 1

HCID 22063454HCID 22063454、化合物

試薬・触媒・溶媒 2

HCID 174Ethylene Glycol溶媒HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ce06c95ba39f48c29ce269d551b1a81a
出典データセット
uspto-grants-2006_06
特許番号
US07056916B2

反応ノート

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