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Diethyl Ether → HCID 178480598, 화합물

HRID 2052068
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반응식

HRID 2052068 반응식
I.[CH3:2][N:3]1[CH:7]=[CH:6][N:5]=[C:4]1[NH:8][C:9](SC)=[N:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.[NH:19]1[CH2:24][CH2:23][O:22][CH2:21][CH2:20]1.CCOCC>CC(O)(C)C>[CH3:2][N:3]1[CH:7]=[CH:6][N:5]=[C:4]1[NH:8][C:9]([N:19]1[CH2:24][CH2:23][O:22][CH2:21][CH2:20]1)=[N:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 3283Diethyl EtherHCID 8083MorpholineHCID 178503857HCID 178503857, 화합물

생성물 1

HCID 178480598HCID 178480598, 화합물

시약·촉매·용매 1

HCID 6386tert-Butanol용매

실험 절차

A solution of 1.5 g (0.004 mole) of methyl N-(1-methylimidazol-2-yl)-N'-phenylcarbamimidothioate hydroiodide and 0.73 g (0.0084 mole) of morpholine in 30 ml of t-BuOH is refluxed overnight. Upon cooling, ether is added and morpholine hydroiodide is removed by filtration. The filtrate is taken to dryness and the residue is taken up in CH2Cl2 and converted to the free base with 3 N NaOH. The organic layer is separated, dried over K2CO3, filtered and the solvent is removed in vacuo to give a residue of N-(1-methylimidazol-2-yl)-N'-phenyl-4-morpholine carboximidamide, which is taken up in acetone and converted to the hydrochloride salt with ethereal HCl.

후처리

  1. temperatureUpon cooling
  2. custommorpholine hydroiodide is removed by filtration
  3. customThe organic layer is separated
  4. dry with materialdried over K2CO3
  5. filtrationfiltered
  6. customthe solvent is removed in vacuo

출처 및 근거

ORD 기록
ord-997af10904894ca4b15c804bffaaa73a
출처 데이터셋
uspto-grants-1980_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04182865

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