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Potassium Iodide → 1-(2-Methoxyethyl)-4-[4-(3-pyrrolidin-1-ylpropoxy)phenyl]piperidine-4-carbonitrile

HRID 273028
ノート
印刷プレビュー

反応式

HRID 273028 の反応式
[N:1]1([CH2:6][CH2:7][CH2:8][O:9][C:10]2[CH:15]=[CH:14][C:13]([C:16]3([C:22]#[N:23])[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]3)=[CH:12][CH:11]=2)[CH2:5][CH2:4][CH2:3][CH2:2]1.Br[CH2:25][CH2:26][O:27][CH3:28].C(=O)(O)[O-].[Na+].[I-].[K+]>C(#N)C>[CH3:28][O:27][CH2:26][CH2:25][N:19]1[CH2:18][CH2:17][C:16]([C:13]2[CH:14]=[CH:15][C:10]([O:9][CH2:8][CH2:7][CH2:6][N:1]3[CH2:5][CH2:4][CH2:3][CH2:2]3)=[CH:11][CH:12]=2)([C:22]#[N:23])[CH2:21][CH2:20]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 4875Potassium IodideHCID 809722-Bromoethyl methyl etherHCID 516892Sodium BicarbonateHCID 598373684-[4-(3-Pyrrolidin-1-ylpropoxy)phenyl]piperidine-4-carbonitrile

生成物 1

HCID 598375241-(2-Methoxyethyl)-4-[4-(3-pyrrolidin-1-ylpropoxy)phenyl]piperidine-4-carbonitrile収率 61%

試薬・触媒・溶媒 1

HCID 6342
Acetonitrile
溶媒

実験手順

A mixture of 4-[4-(3-pyrrolidin-1-ylpropoxy)phenyl]piperidine-4-carbonitrile (68 mg, 0.22 mmol), 2-bromoethylmethylether (21 μl, 0.22 mmol), solid sodium bicarbonate (84 mg, 1.0 mmol) and potassium iodide (5 mg, catalytic) was heated at 50° C. in acetonitrile (1 ml) for 18 hours. The reaction mixture was concentrated in vacuo. The residue was partitioned between dichloromethane (2×50 ml) and 10% aqueous sodium carbonate (20 ml). The organic layers were combined, dried over sodium sulphate, filtered and concentrated in vacuo. The crude product was purified by flash chromatography on silica gel eluting with dichloromethane:methanol:ammonia (97:3:0.3 to 95:5:0.5 by volume) to provide the title compound (46 mg, 61%). 1H NMR (400 MHz, CD3OD) 61.83-1.87 (m, 4H), 2.01-2.10 (m, 6H), 2.45-2.52 (m, 2H), 2.65-2.69 (m, 6H), 2.75 (t, 2H), 3.09 (d, 2H), 3.35 (s, 3H), 3.56 (t, 2H), 4.04 (t, 2H), 6.96 (d, 2H), 7.42 (d, 2H). HRMS ESI+ m/z 372.2639 [MH]+.

後処理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. customThe residue was partitioned between dichloromethane (2×50 ml) and 10% aqueous sodium carbonate (20 ml)
  3. dry with materialdried over sodium sulphate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe crude product was purified by flash chromatography on silica gel eluting with dichloromethane:methanol:ammonia (97:3:0.3 to 95:5:0.5 by volume)

出典と根拠

ORDレコード
ord-67ce5fc3b1654f22bba6e53fde9324e7
出典データセット
uspto-grants-2008_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07456164B2

反応ノート

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