Hydrochloric Acid → 4-amino-1-[2-[N-methyl-N-(tetrahydropyran-4-yl)amino]ethyl]piperidine dihydrochloride

HRID 1169407ノート

反応式

HRID 1169407 の反応式
[CH3:1][N:2]([CH2:9][CH2:10][N:11]1[CH2:16][CH2:15][CH:14]([NH:17]C(=O)OC(C)(C)C)[CH2:13][CH2:12]1)[CH:3]1[CH2:8][CH2:7][O:6][CH2:5][CH2:4]1.[ClH:25]>C(O)C>[ClH:25].[ClH:25].[NH2:17][CH:14]1[CH2:13][CH2:12][N:11]([CH2:10][CH2:9][N:2]([CH3:1])[CH:3]2[CH2:8][CH2:7][O:6][CH2:5][CH2:4]2)[CH2:16][CH2:15]1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 70023872tert-butyl 1-[2-[N-methyl-N-(tetrahydropyran-4-yl)amino]ethyl]-4-piperidinylcarbamate

生成物 1

HCID 229899814-amino-1-[2-[N-methyl-N-(tetrahydropyran-4-yl)amino]ethyl]piperidine dihydrochloride

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Into a solution of tert-butyl 1-[2-[N-methyl-N-(tetrahydropyran-4-yl)amino]ethyl]-4-piperidinylcarbamate (2.72 g) in ethanol (30 ml) was added concentrated hydrochloric acid (10 ml), and the resulting mixture was stirred for 7 hours. After the reaction mixture was concentrated under reduced pressure, ethanol and methanol are added to the residue, and the resulting mixture was concentrated further. The precipitate was collected by filtration and was washed with ethanol and methanol to obtain 4-amino-1-[2-[N-methyl-N-(tetrahydropyran-4-yl)amino]ethyl]piperidine dihydrochloride (1.65 g) as a light yellow powder.

後処理

  1. concentrationAfter the reaction mixture was concentrated under reduced pressure, ethanol and methanol
  2. additionare added to the residue
  3. concentrationthe resulting mixture was concentrated further
  4. filtrationThe precipitate was collected by filtration
  5. washwas washed with ethanol and methanol

出典と根拠

ORDレコード
ord-5a542f1c05824a9bb4f1fd32cd762dce
出典データセット
uspto-grants-2003_09
特許番号
US06627651B1

反応ノート

読み込み中…