Hydrogen chloride-ethyl acetate → 1-(2,3-Dihydro-1,4-benzodioxin-6-ylmethyl)piperidin-4-ylamine

HRID 39720ノート

反応式

HRID 39720 の反応式
[O:1]1[C:6]2[CH:7]=[CH:8][C:9]([CH2:11][N:12]3[CH2:17][CH2:16][CH:15]([NH:18]C(=O)OC(C)(C)C)[CH2:14][CH2:13]3)=[CH:10][C:5]=2[O:4][CH2:3][CH2:2]1.Cl.C(OCC)(=O)C>C(OCC)(=O)C>[O:1]1[C:6]2[CH:7]=[CH:8][C:9]([CH2:11][N:12]3[CH2:17][CH2:16][CH:15]([NH2:18])[CH2:14][CH2:13]3)=[CH:10][C:5]=2[O:4][CH2:3][CH2:2]1

参加物

4

反応物 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 86669946Tert-butyl (1-(2,3-dihydro-1,4-benzodioxin-6-ylmethyl)-piperidin-4-yl)carbamate

生成物 1

HCID 392561291-(2,3-Dihydro-1,4-benzodioxin-6-ylmethyl)piperidin-4-ylamine

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒2 回

実験手順

To 100 mL of an ethyl acetate solution containing 3.62 g of tert-butyl (1-(2,3-dihydro-1,4-benzodioxin-6-ylmethyl)piperidin-4-yl)carbamate, 30 mL of 4 mol/L hydrogen chloride/ethyl acetate was added, and the mixture was stirred at room temperature for 6 hours. The solvent was removed under reduced pressure, the residue thus obtained was added with ethyl acetate, and a solid substance was collected by filtration. The solid substance thus obtained was purified by silica gel column chromatography [silica gel; Chromatorex-NH, manufactured by Fuji Silysia Chemical Ltd., eluent; chloroform:methanol=5:1] to obtain 1.35 g of a pale yellow oily substance, 1-(2,3-dihydro-1,4-benzodioxin-6-ylmethyl)piperidin-4-ylamine.

後処理

  1. additionwas added
  2. customThe solvent was removed under reduced pressure
  3. customthe residue thus obtained
  4. filtrationa solid substance was collected by filtration
  5. customThe solid substance thus obtained
  6. customwas purified by silica gel column chromatography [silica gel; Chromatorex-NH, manufactured by Fuji Silysia Chemical Ltd., eluent; chloroform:methanol=5:1]

出典と根拠

ORDレコード
ord-cd911618ac7f435690993a9c407ee8bb
出典データセット
uspto-grants-2013_09
特許番号
US08524738B2

反応ノート

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