Hydrochloric Acid → HCID 23000985、化合物

HRID 397742ノート

反応式

HRID 397742 の反応式
[CH2:1]([N:7]1[CH2:12][CH2:11][CH:10]([C:13]2[CH:18]=[CH:17][CH:16]=[C:15]([NH:19]C(=O)C(O)(C)C)[CH:14]=2)[CH2:9][CH2:8]1)[CH2:2][CH2:3][CH2:4][CH2:5][CH3:6].Cl>O1CCOCC1.O>[NH2:19][C:15]1[CH:14]=[C:13]([CH:10]2[CH2:11][CH2:12][N:7]([CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH3:6])[CH2:8][CH2:9]2)[CH:18]=[CH:17][CH:16]=1

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 23001068HCID 23001068、化合物

生成物 1

HCID 23000985HCID 23000985、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 312751,4-Dioxane溶媒

実験手順

A solution of N-hexyl-4-(3-(2-hydroxy-2-methylpropanoylamino)phenyl)piperidine (Example 158) in 1,4-dioxan:5N aqueous hydrochloric acid solution (1:1, 10 ml) was heated under reflux overnight. The reaction mixture was cooled, diluted with water (10 ml) and extracted with diethyl ether (3×10 ml). The pH of the aqueous layer was adjusted to 8-9 using 5N aqueous sodium hydroxide, and extracted with dichloromethane (5×10 ml). The combined extracts were washed with brine (10 ml), dried (Na2SO4) and concentrated in vacuo to give the title compound as an oil which was not purified further (178 mg, 61% over two steps).

後処理

  1. temperatureunder reflux overnight
  2. temperatureThe reaction mixture was cooled
  3. extractionextracted with diethyl ether (3×10 ml)
  4. extractionextracted with dichloromethane (5×10 ml)
  5. washThe combined extracts were washed with brine (10 ml)
  6. dry with materialdried (Na2SO4)
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-5cba0c1961d44f6790a509783b3bd4b5
出典データセット
uspto-grants-2003_08
特許番号
US06610711B2

反応ノート

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