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Hydrochloric Acid → 1-(4-Fluoro-3-methylphenyl)-2-methylpropan-2-amine

HRID 506555
ノート
印刷プレビュー

反応式

HRID 506555 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]([NH:12]C=O)([CH3:11])[CH3:10])=[CH:4][C:3]=1[CH3:15].Cl.[OH-].[Na+]>O>[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]([NH2:12])([CH3:10])[CH3:11])=[CH:4][C:3]=1[CH3:15]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 22063477HCID 22063477、化合物

生成物 1

HCID 220634761-(4-Fluoro-3-methylphenyl)-2-methylpropan-2-amine

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

4.3 g (20.6 mmol) of N-[2-(4-fluoro-3-methylphenyl)-1,1-dimethylethyl]formamide, 20 mL concentrated hydrochloric acid, and 20 mL water are refluxed for 2 hours. The reaction mixture is diluted with water, made alkaline with concentrated sodium hydroxide solution, and extracted with dichloromethane. The organic phases are dried with sodium sulfate and evaporated down. The residue is dissolved in ethyl acetate, combined with ethereal hydrochloric acid, and cooled. The crystals precipitated are suction filtered and washed with diethyl ether and dried. White solid. Yield: 3.9 g (87%, hydrochloride); melting point 196° C.-198° C.

後処理

  1. extractionextracted with dichloromethane
  2. dry with materialThe organic phases are dried with sodium sulfate
  3. customevaporated down
  4. dissolutionThe residue is dissolved in ethyl acetate
  5. temperaturecooled
  6. customThe crystals precipitated
  7. filtrationare suction filtered
  8. washwashed with diethyl ether
  9. customdried

出典と根拠

ORDレコード
ord-7c38694f33594d41b8d0446364b88b8e
出典データセット
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07786111B2

反応ノート

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