Hydrochloric Acid → 5-Azaspiro[2.4]heptan-7-ol hydrochloride
反応式
C1(C[N:8]2[CH2:14][CH:13]([OH:15])[C:10]3([CH2:12][CH2:11]3)[CH2:9]2)C=CC=CC=1.[ClH:16]>CO>[ClH:16].[CH2:11]1[C:10]2([CH:13]([OH:15])[CH2:14][NH:8][CH2:9]2)[CH2:12]1参加物
4
実験手順
5-(Phenylmethyl)-5-azaspiro[2.4]heptan-7-ol (assumed 941.9 mg, 4.63 mmol) was dissolved in a solution of 4.6 mL of 1N aq HCl in 40 mL of MeOH, degassed and placed under argon. 10% Pd/C (280 mg) was added, and the contents were thoroughly degassed and placed under a hydrogen balloon overnight. The contents were then degassed and filtered through Celite, and the Celite pad was washed with MeOH. The resulting filtrate was concentrated in vacuo and azeotroped with MeOH (3×40 mL) to provide the pure 5-azaspiro[2.4]heptan-7-ol hydrochloride (685 mg, 99%). LCMS: (M+H)+: not detected.
後処理
- customdegassed
- addition10% Pd/C (280 mg) was added
- customthe contents were thoroughly degassed
- customballoon overnight
- customThe contents were then degassed
- filtrationfiltered through Celite
- washthe Celite pad was washed with MeOH
- concentrationThe resulting filtrate was concentrated in vacuo
- customazeotroped with MeOH (3×40 mL)
出典と根拠
- ORDレコード
- ord-1308249cba8b48dd96002798cd011088
- 出典データセット
- uspto-grants-2011_02
- 特許番号
- US07893056B2
反応ノート
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