Trifluoroacetic acid → 1-(2-Methoxyethyl)piperidin-4-amine

HRID 271517

反応式

HRID 271517 の反応式
[CH3:1][O:2][CH2:3][CH2:4][N:5]1[CH2:10][CH2:9][CH:8]([NH:11]CC2OC(C3C=C4C(=CC=3)C(=NO)CC4)=C(C3C=CN=CC=3)C=2)[CH2:7][CH2:6]1.FC(F)(F)C(O)=O>ClCCl>[CH3:1][O:2][CH2:3][CH2:4][N:5]1[CH2:6][CH2:7][CH:8]([NH2:11])[CH2:9][CH2:10]1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 1363552505-(5-{[1-(2-Methoxy-ethyl)-piperidin-4-ylamino]-methyl}-3-pyridin-4-yl-furan-2-yl)-indan-1-one oxime

生成物 1

HCID 201191211-(2-Methoxyethyl)piperidin-4-amine収率 47.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of the product from Step 1 (500 mg, 1.94 mmol) in dichloromethane (5 ml) was cooled to 0° C. and treated with trifluoroacetic acid (2 ml). The mixture was allowed to warm to room temperature and stirred for a further 1 hour. After evaporation of the solvent in vacuo, the residue was partitioned between dichloromethane and an aqueous solution of sodium carbonate. After separation of the layers the aqueous phase was re-extracted six times with dichloromethane, dried and concentrated in vacuo to yield the title compound (145 mg, 47%); 1H NMR (CD3OD) 3.49 (2H, t, J 5.2 Hz), 3.35 (3H, s), 3.30 (2H, m), 3.10 (1H, s), 2.80 (2H, t, J 5.2 Hz), 2.68 (2H, m), 1.91 (2H, m), 1.30 (2H, m).

後処理

  1. customAfter evaporation of the solvent in vacuo
  2. customthe residue was partitioned between dichloromethane
  3. customAfter separation of the layers the aqueous phase
  4. extractionwas re-extracted six times with dichloromethane
  5. customdried
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-306320b3575645a596b9f091b69719b5
出典データセット
uspto-grants-2008_11
特許番号
US07452906B2

関連ノート

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