Iodoethane → 3-(3,4-Difluorophenyl)-1-ethyl-3-methoxypyrrolidine

HRID 575954ノート

反応式

HRID 575954 の反応式
[F:1][C:2]1[CH:3]=[C:4]([C:9]2([O:14][CH3:15])[CH2:13][CH2:12][NH:11][CH2:10]2)[CH:5]=[CH:6][C:7]=1[F:8].[CH2:16](N(CC)CC)[CH3:17].ICC>O1CCCC1>[F:1][C:2]1[CH:3]=[C:4]([C:9]2([O:14][CH3:15])[CH2:13][CH2:12][N:11]([CH2:16][CH3:17])[CH2:10]2)[CH:5]=[CH:6][C:7]=1[F:8]

参加物

5

反応物 3

HCID 6340IodoethaneHCID 8471TriethylamineHCID 462192213-(3,4-Difluorophenyl)-3-methoxypyrrolidine

生成物 1

HCID 462192223-(3,4-Difluorophenyl)-1-ethyl-3-methoxypyrrolidine

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of (−)-3-(3,4-difluorophenyl)-3-methoxypyrrolidine (0.013 g, 0.061 mmol) and triethylamine (17.1 μL, 0.122 mmol) in tetrahydrofuran (2 ml), was added iodoethane (7.3 μL, 0.091 mmol), the resulting solution was stirred at ambient temperature for 24 h. The crude mixture was purified on a Biotage Isolute SCX-3 SPE column (washed with methanol and eluted with methanol/triethylamine, 4:1). The solvent was evaporated and the crude product was analyzed by GCMS. Analysis showed 76% conversion. MS m/z (relative intensity, 70 eV) 241 (M+, 7), 226 (57), 211 (24), 141 (43), 71 (bp).

後処理

  1. customThe crude mixture was purified on a Biotage Isolute SCX-3 SPE column (washed with methanol and eluted with methanol/triethylamine, 4:1)
  2. customThe solvent was evaporated

出典と根拠

ORDレコード
ord-a7d933e239f1421ca983fa592fdd1875
出典データセット
uspto-grants-2015_05
特許番号
US09035073B2

反応ノート

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