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Sodium Iodide → HCID 68468406, 화합물

HRID 506785
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HRID 506785 반응식
Cl[CH2:2][CH2:3][N:4]1[C:12]2[C:7](=[N:8][C:9]([O:15][CH3:16])=[C:10]([O:13][CH3:14])[CH:11]=2)[C:6]([C:17]2[N:26]([S:27]([C:30]3[CH:35]=[CH:34][C:33]([CH3:36])=[CH:32][CH:31]=3)(=[O:29])=[O:28])[C:20]3=[N:21][CH:22]=[CH:23][C:24]([Cl:25])=[C:19]3[CH:18]=2)=[CH:5]1.[Na+].[I-:38]>CC(=O)CC>[Cl:25][C:24]1[CH:23]=[CH:22][N:21]=[C:20]2[N:26]([S:27]([C:30]3[CH:31]=[CH:32][C:33]([CH3:36])=[CH:34][CH:35]=3)(=[O:29])=[O:28])[C:17]([C:6]3[C:7]4=[N:8][C:9]([O:15][CH3:16])=[C:10]([O:13][CH3:14])[CH:11]=[C:12]4[N:4]([CH2:3][CH2:2][I:38])[CH:5]=3)=[CH:18][C:19]=12
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 5238Sodium IodideHCID 68469439HCID 68469439, 화합물

생성물 1

HCID 68468406HCID 68468406, 화합물수율 96.6%

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

실험 절차

Dissolve chlorobisazaindole 31 (110 mg, 0.202 mmol) and NaI (33.5 mg, 0.222 mmol) in 2-butanone (10 mL) and reflux for 24 h. The reaction medium is then concentrated under vacuum, the residue is dissolved in EtOAc, washed with brine, dried (Na2SO4) and concentrated, to give 32 (124 mg, 96.6%) as a yellow solid: 1H NMR (CDCl3) δ 8.25 (d, 1H, J=5.4 Hz), 7.71 (d, 2H, J=8.4 Hz), 7.65 (s, 1H), 7.10 (m, 5H), 4.53 (t, 2H, J=6.4 Hz), 4.03 (s, 3H), 3.99 (s, 3H), 3.50 (t, 2H, J=6.4 Hz), 2.31 (s, 3H), TLC (EtOAc at 40%/heptane) Rf=0.20, m/z obs.=636.9 (M+1), 638.9, 639.94.

후처리

  1. temperaturereflux for 24 h
  2. concentrationThe reaction medium is then concentrated under vacuum
  3. dissolutionthe residue is dissolved in EtOAc
  4. washwashed with brine
  5. dry with materialdried (Na2SO4)
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-b94d7033dd5e4453857cdde2d5923790
출처 데이터셋
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07786114B2

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