Potassium Carbonate → HCID 25143671, 화합물

HRID 1931811노트

반응식

HRID 1931811 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 25143671HCID 25143671, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-5d4bcd40cb454c579ba1b32305ac27ff
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08188301B2

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