Methanol → Methyl 4-aminooxane-4-carboxylate hydrochloride

HRID 383536

反応式

HRID 383536 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-caa6434e25514b198f46e5a096eb539c
出典データセット
uspto-grants-2013_02
特許番号
US08367666B2

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