Methanol → Methyl 4-aminooxane-4-carboxylate hydrochloride

HRID 1925627

反応式

HRID 1925627 の反応式
S(Cl)([Cl:3])=O.Cl.[NH2:6][C:7]1([C:13]([OH:15])=[O:14])[CH2:12][CH2:11][O:10][CH2:9][CH2:8]1.[CH3:16]O>>[ClH:3].[NH2:6][C:7]1([C:13]([O:15][CH3:16])=[O:14])[CH2:12][CH2:11][O:10][CH2:9][CH2:8]1

参加物

4

反応物 3

HCID 887MethanolHCID 24386Thionyl ChlorideHCID 27344004-Aminotetrahydro-2H-pyran-4-carboxylic acid hydrochloride

生成物 1

HCID 43811077Methyl 4-aminooxane-4-carboxylate hydrochloride

実験手順

Thionyl chloride (4.02 mL, 55.1 mmol) was added in the dehydrated methanol (100 mL) solution of 4-amino-4-carboxytetrahydro-pyran monohydrochloride (5.00 g, 27.5 mmol) in an ice bath, and the mixture was heated and refluxed for 2.5 hours. The solvent was removed by distillation under reduced pressure, and the obtained crude product was washed with ethyl acetate and then dried under reduced pressure to give a colorless solid (BB04, 5.06 g).

後処理

  1. temperaturethe mixture was heated
  2. temperaturerefluxed for 2.5 hours
  3. customThe solvent was removed by distillation under reduced pressure
  4. customthe obtained crude product
  5. washwas washed with ethyl acetate
  6. customdried under reduced pressure
  7. customto give a colorless solid (BB04, 5.06 g)

出典と根拠

ORDレコード
ord-7ecba03d30d747bcb75ea1f42743ff81
出典データセット
uspto-grants-2012_05
特許番号
US08178681B2

関連ノート

読み込み中…