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Hydrochloric Acid → 3-Fluoro-1-(1-tosyl-5-imidazolyl)propan-2-ol

HRID 27612
ノート
印刷プレビュー

反応式

HRID 27612 の反応式
[F:1][CH2:2][C:3]([CH2:5][C:6]1[N:10]([S:11]([C:14]2[CH:20]=[CH:19][C:17]([CH3:18])=[CH:16][CH:15]=2)(=[O:13])=[O:12])[CH:9]=[N:8][CH:7]=1)=[O:4].[BH4-].[Na+].Cl>CO>[F:1][CH2:2][CH:3]([OH:4])[CH2:5][C:6]1[N:10]([S:11]([C:14]2[CH:15]=[CH:16][C:17]([CH3:18])=[CH:19][CH:20]=2)(=[O:13])=[O:12])[CH:9]=[N:8][CH:7]=1
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 4311764Sodium borohydrideHCID 23343259HCID 23343259、化合物

生成物 1

HCID 233432033-Fluoro-1-(1-tosyl-5-imidazolyl)propan-2-ol

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of 20 mmole of 1-tosyl-5-imidazolylmethyl fluoromethyl ketone in 25 ml of methanol cooled to -10° C. is treated with 30 mg of sodium borohydride. After two hours at from -10° to 0° C. the reaction mixture is neutralized with 6 M HCl and concentrated under vacuo. The residue is extracted several times with chloroform. Evaporation of the solvent affords an oil which is purified by distillation under high vacuum to give 3-fluoro-1-(1-tosyl-5-imidazolyl)propan-2-ol. A solution of 2 g of 3-fluoro-1-(1-tosyl-5-imidazolyl)propan-2-ol, 1.37 g of phthalimide, 1.74 g of diethylazodicarboxylate in 2.4 g of triphenylphosphine and 25 ml of tetrahydrofuran is stirred under nitrogen at 25° C. for 20 hours after which the solvent is evaporated at reduced pressure and the residue is taken up in benzene. The insoluble material is discarded and the semi-solid residue obtained after concentration of the filtrate under vacuum is recrystallized using dichloromethane/diethylether to give the fluorophthalimide derivative. A solution of 1.12 g of the fluorophthalimide derivative in 0.18 g of hydrazine hydrate in 42 ml of absolute ethanol is heated at reflux for 5 hours. Upon cooling the solution is concentrated under vacuum to a volume of 15 ml, allowed to stand overnight at 0° C. then filtered. The filtrate is concentrated and distilled under high vacuum to afford 1-fluoromethyl-2-(1-tosyl-5-imidazolyl)ethylamine which is combined with 6 ml of 47% hydrogen bromide and heated under nitrogen at 100° C. for 4 hours then concentrated under reduced pressure to give a solid residue. The residue is recrystallized from ethanol-diethylether to give 1-fluoromethyl-2-(5-imidazolyl)ethylamine hydrobromide.

後処理

  1. concentrationconcentrated under vacuo
  2. extractionThe residue is extracted several times with chloroform
  3. customEvaporation of the solvent
  4. customaffords an oil which
  5. distillationis purified by distillation under high vacuum

出典と根拠

ORDレコード
ord-e96477738df4447794aab557f784e5f7
出典データセット
uspto-grants-1980_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04221914

反応ノート

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