Potassium Carbonate → HCID 25143671、化合物

HRID 1931811

反応式

HRID 1931811 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C:9]2([OH:14])[CH2:13][CH2:12][NH:11][CH2:10]2)[CH:5]=[CH:6][C:7]=1[F:8].C(=O)([O-])[O-].[K+].[K+].I[CH2:22][CH2:23][CH3:24]>C(#N)C>[Cl:1][C:2]1[CH:3]=[C:4]([C:9]2([OH:14])[CH2:13][CH2:12][N:11]([CH2:22][CH2:23][CH3:24])[CH2:10]2)[CH:5]=[CH:6][C:7]=1[F:8]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 336431-IodopropaneHCID 685178373-(3-Chloro-4-fluorophenyl)pyrrolidin-3-ol

生成物 1

HCID 25143671HCID 25143671、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

Preparation according to Example 22: 3-(3-chloro-4-fluorophenyl)pyrrolidin-3-ol (0.8 g, 3.72 mmol), potassium carbonate (1.03 g, 7.45 mmol), iodopropane (0.83 mg, 4.86 mmol), acetonitrile (20 mL). Purification by flash chromatography on silica gel (ethyl acetate/methanol, 1:1 to 0:1). Yield: 520 mg. The amine was converted to the fumaric acid salt and recrystallized from ethanol/diethyl ether: M.p. 157.9° C.; MS m/z (relative intensity, 70 eV) 257 (M+, 8), 228 (bp), 198 (30), 157 (15), 84 (88).

後処理

  1. customPreparation
  2. customPurification by flash chromatography on silica gel (ethyl acetate/methanol, 1:1 to 0:1)
  3. customrecrystallized from ethanol/diethyl ether

出典と根拠

ORDレコード
ord-5d4bcd40cb454c579ba1b32305ac27ff
出典データセット
uspto-grants-2012_05
特許番号
US08188301B2

関連ノート

読み込み中…