N-Cyclopropylmethyl-N-(2-ethyl-7-iodopyrazolo[1,5-a]pyridin-3-yl)-N-tetrahydro-2H-4-pyranylmethylamine hydrochloride → N-Cyclopropylmethyl-2-ethyl-7-iodo-N-(tetrahydro-2H-pyran-4-ylmethyl)pyrazolo[1,5-a]pyridine-3-amine

HRID 2267198ノート

反応式

HRID 2267198 の反応式
Cl.[CH:2]1([CH2:5][N:6]([CH2:19][CH:20]2[CH2:25][CH2:24][O:23][CH2:22][CH2:21]2)[C:7]2[C:8]([CH2:17][CH3:18])=[N:9][N:10]3[C:15]([I:16])=[CH:14][CH:13]=[CH:12][C:11]=23)[CH2:4][CH2:3]1.O.C(=O)(O)[O-].[Na+]>C(OCC)(=O)C>[CH:2]1([CH2:5][N:6]([CH2:19][CH:20]2[CH2:21][CH2:22][O:23][CH2:24][CH2:25]2)[C:7]2[C:8]([CH2:17][CH3:18])=[N:9][N:10]3[C:15]([I:16])=[CH:14][CH:13]=[CH:12][C:11]=23)[CH2:4][CH2:3]1

参加物

4

反応物 2

HCID 21084143N-Cyclopropylmethyl-N-(2-ethyl-7-iodopyrazolo[1,5-a]pyridin-3-yl)-N-tetrahydro-2H-4-pyranylmethylamine hydrochlorideHCID 86585896Sodium bicarbonate water

生成物 1

HCID 11339625N-Cyclopropylmethyl-2-ethyl-7-iodo-N-(tetrahydro-2H-pyran-4-ylmethyl)pyrazolo[1,5-a]pyridine-3-amine収率 88%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

To N-cyclopropylmethyl-2-ethyl-7-iodo-N-(tetrahydro-2H-pyran-4-ylmethyl)pyrazolo[1,5-a]pyridine-3-amine hydrochloride (16 g) was added saturated sodium bicarbonate water (200 mL) to give neutrality. Then, ethyl acetate (100 mL) was added to this, and an organic layer was separated. From the organic layer, the solvent was distilled off under reduced pressure. Into the resulting residue was dropped acetonitrile (30 mL) and water (120 mL), the mixture was stirred overnight, and the resulting precipitate was filtrated. The precipitate was dried under reduced pressure, and 13 g of a title compound was obtained as white crystal.

後処理

  1. customto give neutrality
  2. customwas separated
  3. distillationFrom the organic layer, the solvent was distilled off under reduced pressure
  4. additionInto the resulting residue was dropped acetonitrile (30 mL) and water (120 mL)
  5. filtrationthe resulting precipitate was filtrated
  6. customThe precipitate was dried under reduced pressure

出典と根拠

ORDレコード
ord-b19a3fbd708d468ea5ce281b5fdcec74
出典データセット
uspto-grants-2010_12
特許番号
US07858809B2

反応ノート

読み込み中…