Methyl iodide → HCID 21251015, 화합물

HRID 1531844노트

반응식

HRID 1531844 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]1[CH2:13][CH2:12][NH:11][C:10]1=[S:14].[H-].[Na+].[CH3:17]I>CN(C)C=O>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]1[CH:13]=[CH:12][N:11]=[C:10]1[S:14][CH3:17]

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 570963221-(2-Methoxyphenyl)-2-imidazolidinethione

생성물 1

HCID 21251015HCID 21251015, 화합물수율 100.1%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매3회

반응 조건

온도
0 °C

실험 절차

A solution of 8.1 g (0.039 mol) of this 1-(2-methoxyphenyl)imidazoline-2-thione in 88 ml of dimethylformamide is added dropwise, under nitrogen at 0° C., to a suspension of 1.19 g (0.047 mol) of sodium hydride (95%) in 88 ml of anhydrous dimethylformamide. The reaction mixture is stirred for ¾ h at 0° C. 2.7 ml (0.043 mol) of methyl iodide previously diluted in 24 ml of dimethylformamide are added and the mixture is stirred for 1 hour at 0° C. The reaction mixture is poured over ice, extracted three times with ethyl acetate and washed twice with water and then with brine. The product is dried over magnesium sulphate, filtered and concentrated. 8.6 g of oil are obtained.

후처리

  1. additionare added
  2. stirringthe mixture is stirred for 1 hour at 0° C
  3. additionThe reaction mixture is poured over ice
  4. extractionextracted three times with ethyl acetate
  5. washwashed twice with water
  6. dry with materialThe product is dried over magnesium sulphate
  7. filtrationfiltered
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-575d18994a004fda81191a99c31e7bf4
출처 데이터셋
uspto-grants-2001_03
특허 번호
US06200991B1

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