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Sodium Iodide → HCID 19698534, 화합물

HRID 862554
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HRID 862554 반응식
[NH2:1][C:2]1[C:3]2[N:4]([C:8]([CH:12]=[O:13])=[C:9]([CH3:11])[N:10]=2)[CH:5]=[CH:6][CH:7]=1.C(=O)([O-])[O-].[Na+].[Na+].[I-].[Na+].Cl[CH2:23][C:24]1[C:29]([CH3:30])=[CH:28][CH:27]=[CH:26][C:25]=1[NH:31][C:32](=[O:38])[O:33][CH2:34][CH2:35][O:36][CH3:37]>CC(C)=O>[CH3:37][O:36][CH2:35][CH2:34][O:33][C:32]([NH:31][C:25]1[CH:26]=[CH:27][CH:28]=[C:29]([CH3:30])[C:24]=1[CH2:23][NH:1][C:2]1[C:3]2[N:4]([C:8]([CH:12]=[O:13])=[C:9]([CH3:11])[N:10]=2)[CH:5]=[CH:6][CH:7]=1)=[O:38]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 5238Sodium IodideHCID 10340Sodium CarbonateHCID 21873989HCID 21873989, 화합물HCID 538354172-Methoxyethyl 2-chloromethyl-3-methylphenylcarbamate

생성물 1

HCID 19698534HCID 19698534, 화합물수율 73.2%

시약·촉매·용매 1

HCID 180Acetone
용매

실험 절차

A mixture of 2.0 g (11.41 mmol) of 8-amino-2-methylimidazo[1,2-a]pyridine-3-carboxaldehyde, 1.21 g (11.41 mmol) of anhydrous sodium carbonate, 0.17 g (1.14 mmol) of sodium iodide and 3.5 g (13.6 mmol) of 2-methoxyethyl 2-chloromethyl-3-methylphenylcarbamate in 30 ml of acetone is stirred at RT for 24 h and concentrated in a Rotavapor. The residue is treated with 100 ml of water and extracted with ethyl acetate, and the organic phase is dried with magnesium sulphate and concentrated in vacuo. The residue is recrystallized from toluene. 3.31 g (73%) of the title compound of m.p. 153°-155° C. are obtained.

후처리

  1. concentrationconcentrated in a Rotavapor
  2. additionThe residue is treated with 100 ml of water
  3. extractionextracted with ethyl acetate
  4. dry with materialthe organic phase is dried with magnesium sulphate
  5. concentrationconcentrated in vacuo
  6. customThe residue is recrystallized from toluene

출처 및 근거

ORD 기록
ord-6ffeecee329f4fb5ab07bccd4fac3471
출처 데이터셋
uspto-grants-1998_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05719161

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