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

HRID 39720노트

반응식

HRID 39720 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

실험 절차

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.

후처리

  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]

출처 및 근거

ORD 기록
ord-cd911618ac7f435690993a9c407ee8bb
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08524738B2

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