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tert-Butyl 3-(4-{[(1-adamantylmethyl)amino]carbonyl}-5-chloropyridin-2-yl)propyl[3-(tetrahydro-2H-pyran-2-yloxy)propyl]carbamate → N-(1-Adamantylmethyl)-5-chloro-2-{3-[(3-hydroxypropyl)amino]propyl}isonicotinamide dihydrochloride

HRID 1247585
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HRID 1247585 반응식
[C:1]12([CH2:11][NH:12][C:13]([C:15]3[C:20]([Cl:21])=[CH:19][N:18]=[C:17]([CH2:22][CH2:23][CH2:24][N:25]([CH2:33][CH2:34][CH2:35][O:36]C4CCCCO4)C(=O)OC(C)(C)C)[CH:16]=3)=[O:14])[CH2:10][CH:5]3[CH2:6][CH:7]([CH2:9][CH:3]([CH2:4]3)[CH2:2]1)[CH2:8]2>CO.Cl>[ClH:21].[ClH:21].[C:1]12([CH2:11][NH:12][C:13](=[O:14])[C:15]3[C:20]([Cl:21])=[CH:19][N:18]=[C:17]([CH2:22][CH2:23][CH2:24][NH:25][CH2:33][CH2:34][CH2:35][OH:36])[CH:16]=3)[CH2:8][CH:7]3[CH2:9][CH:3]([CH2:4][CH:5]([CH2:6]3)[CH2:10]1)[CH2:2]2
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반응물 1

HCID 86595926tert-Butyl 3-(4-{[(1-adamantylmethyl)amino]carbonyl}-5-chloropyridin-2-yl)propyl[3-(tetrahydro-2H-pyran-2-yloxy)propyl]carbamate

생성물 1

HCID 21906713N-(1-Adamantylmethyl)-5-chloro-2-{3-[(3-hydroxypropyl)amino]propyl}isonicotinamide dihydrochloride수율 176.2%

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 887Methanol용매

실험 절차

tert-Butyl 3-(4-{[(1-adamantylmethyl)amino]carbonyl}-5-chloropyridin-2-yl)propyl[3-(tetrahydro-2H-pyran-2-yloxy)propyl]carbamate (Example 2(iv)) (0.24 g) was dissolved in a mixture of methanol (10 ml) and 2M aqueous hydrochloric acid solution (10 ml); the solution was left to stand for 0.5 hours. The mixture was concentrated and the residue diluted with 2M aqueous sodium hydroxide solution (25 ml). The mixture was extracted into dichloromethane (3×25 ml) and the combined extracts were concentrated. The residue was dissolved in a solution of hydrogen chloride in 1,4-dioxane (10 ml of a 4M solution) and left to stand for 0.5 hours. The solution was concentrated and the residue suspended in 2M aqueous sodium hydroxide solution (25 ml), extracted into dichloromethane (3×25 ml) and the combined extracts were concentrated. The residue was purified by chromatography on silica gel eluting with dichloromethane:methanol:0.88 aqueous ammonia (89:10:1). The isolated material was dissolved in a solution of hydrogen chloride in 1,4-dioxane (10 ml of a 4M solution) and concentrated; the resultant solid was recrystallised from ethyl acetate/methanol to afford the titled compound (0.115 g) as a colourless solid.

후처리

  1. waitthe solution was left
  2. concentrationThe mixture was concentrated
  3. additionthe residue diluted with 2M aqueous sodium hydroxide solution (25 ml)
  4. extractionThe mixture was extracted into dichloromethane (3×25 ml)
  5. concentrationthe combined extracts were concentrated
  6. dissolutionThe residue was dissolved in a solution of hydrogen chloride in 1,4-dioxane (10 ml of a 4M solution) and
  7. waitleft
  8. waitto stand for 0.5 hours
  9. concentrationThe solution was concentrated
  10. extractionextracted into dichloromethane (3×25 ml)
  11. concentrationthe combined extracts were concentrated
  12. customThe residue was purified by chromatography on silica gel eluting with dichloromethane
  13. dissolutionThe isolated material was dissolved in a solution of hydrogen chloride in 1,4-dioxane (10 ml of a 4M solution) and
  14. concentrationconcentrated
  15. customthe resultant solid was recrystallised from ethyl acetate/methanol

출처 및 근거

ORD 기록
ord-a11e0c794dc8463e97b91c8f732f15ae
출처 데이터셋
uspto-grants-2006_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07129246B2

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