2-Chloroethyl chloroformate → 5-Methyl-1,4-oxazepane hydrochloride

HRID 515445ノート

反応式

HRID 515445 の反応式
C([N:8]1[CH:14]([CH3:15])[CH2:13][CH2:12][O:11][CH2:10][CH2:9]1)C1C=CC=CC=1.[Cl:16]C(OCCCl)=O>ClCCCl>[ClH:16].[CH3:15][CH:14]1[CH2:13][CH2:12][O:11][CH2:10][CH2:9][NH:8]1

参加物

4

反応物 2

HCID 123052-Chloroethyl chloroformateHCID 667187904-Benzyl-5-methyl-[1,4]oxazepane

生成物 1

HCID 667186395-Methyl-1,4-oxazepane hydrochloride収率 78.6%

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

実験手順

To a solution of 4-benzyl-5-methyl-[1,4]oxazepane (0.30 g, 1.4 mmol) in 1,2-dichloroethane (3 mL) was added chloroethyl chloroformate (0.56 mL, 7 mmol) at room temperature. The mixture was refluxed for 10 hours and concentrated. The resulting residue was dissolved in methanol (5 mL) and the solution was refluxed for one hour. After concentration, the residual material was triturated, washed with ethyl acetate and collected by filtration to afford 5-methyl-[1,4]oxazepane hydrochloride (0.16 g, 1.1 mmol, 76%) as a white solid.

後処理

  1. temperatureThe mixture was refluxed for 10 hours
  2. concentrationconcentrated
  3. dissolutionThe resulting residue was dissolved in methanol (5 mL)
  4. temperaturethe solution was refluxed for one hour
  5. concentrationAfter concentration
  6. customthe residual material was triturated
  7. washwashed with ethyl acetate
  8. filtrationcollected by filtration

出典と根拠

ORDレコード
ord-337a7b879283470cba51f99f8306b20f
出典データセット
uspto-grants-2015_08
特許番号
US09108957B2

反応ノート

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