N-Iodosuccinimide → HCID 22050117, 화합물

HRID 1831901노트

반응식

HRID 1831901 반응식
[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][N:12]([CH2:15][C:16]2[CH:21]=[CH:20][CH:19]=[C:18]([F:22])[CH:17]=2)[C:11](=[O:23])[CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[I:24]N1C(=O)CCC1=O>C(#N)C>[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][N:12]([CH2:15][C:16]2[CH:21]=[CH:20][CH:19]=[C:18]([F:22])[CH:17]=2)[C:11](=[O:23])[C:10]=1[I:24])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 120273N-IodosuccinimideHCID 220502224-benzyloxy-1-(3-fluorobenzyl)-1H-pyridin-2-one

생성물 1

HCID 22050117HCID 22050117, 화합물수율 90.6%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

Heated a reaction mixture of 4-(benzyloxy)-1-(3-fluorobenzyl)pyridin-2(1H)-one (4.83 g, 15.6 mmol) in anhydrous acetonitrile (55 mL) and N-iodosuccinimide (NIS, 3.86 g, 17.1 mmol) under nitrogen atmosphere at 650 C for 4 h. The reaction mixture was concentrated under reduced pressure and the residue was purified by flash chromatography (silica gel) using EtOAc/hexanes (1:1 v:v). The appropriate fractions were collected according to ES MS (M+H 436) and washed with Na2SO3 to remove the color impurities. The fractions were concentrated under reduced pressure and dried in vacuo to afford the desired product (6.15 g, 90%) as a light yellow solid.

후처리

  1. temperatureHeated
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. customthe residue was purified by flash chromatography (silica gel)
  4. customThe appropriate fractions were collected
  5. washwashed with Na2SO3
  6. customto remove the color impurities
  7. concentrationThe fractions were concentrated under reduced pressure
  8. customdried in vacuo

출처 및 근거

ORD 기록
ord-ec539c599c0d411f8ec888a3ccce30f8
출처 데이터셋
uspto-grants-2006_06
특허 번호
US07067540B2

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