N-Iodosuccinimide → 2-(1-bromopropyl)-3-iodo-6-methyl-4H-pyrido[1,2-a]pyrimidin-4-one

HRID 58224

반응식

HRID 58224 반응식
[Br:1][CH:2]([C:5]1[N:6]=[C:7]2[CH:15]=[CH:14][CH:13]=[C:12]([CH3:16])[N:8]2[C:9](=[O:11])[CH:10]=1)[CH2:3][CH3:4].[I:17]N1C(=O)CCC1=O>C(#N)C>[Br:1][CH:2]([C:5]1[N:6]=[C:7]2[CH:15]=[CH:14][CH:13]=[C:12]([CH3:16])[N:8]2[C:9](=[O:11])[C:10]=1[I:17])[CH2:3][CH3:4]

참가 물질

4

반응물 2

HCID 120273N-IodosuccinimideHCID 668642082-(1-bromopropyl)-6-methyl-4H-pyrido[1,2-a]pyrimidin-4-one

생성물 1

HCID 668641442-(1-bromopropyl)-3-iodo-6-methyl-4H-pyrido[1,2-a]pyrimidin-4-one수율 90.5%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
80 °C

실험 절차

A mixture of 2-(1-bromopropyl)-6-methyl-4H-pyrido[1,2-a]pyrimidin-4-one (3.46 g, 12.3 mmol) and N-iodosuccinimide (4.15 g, 18.4 mmol) in acetonitrile (100 mL) was stirred at 80° C., under nitrogen, overnight. After removal of acetonitrile in vacuum, the resulting solid was dissolved in methylene chloride, washed with water, saturated Na2S2O3, saturated sodium bicarbonate, and brine; and then the organic layers dried over sodium sulfate and then filtered. The filtrate was concentrated under reduced pressure to provide the desired product (4.53 g, 90.4%). LCMS calculated for C12H13BrIN2O (M+H)+: m/z=406.9. Found: 407.1.

후처리

  1. customAfter removal of acetonitrile in vacuum
  2. dissolutionthe resulting solid was dissolved in methylene chloride
  3. washwashed with water, saturated Na2S2O3, saturated sodium bicarbonate, and brine
  4. dry with materialand then the organic layers dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationThe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-a1a37df2a7c047c4a48b07db83119876
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09434746B2

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