Carbofuran → Glycine, N-(((((2,3-dihydro-2,2-dimethyl-7-benzofuranyl)oxy)carbonyl)methylamino)thio)-N-(2-ethoxy-2-oxoethyl)-, ethyl ester

HRID 1648755

반응식

HRID 1648755 반응식
[CH3:1][NH:2][C:3](=[O:16])[O:4][C:5]1[C:13]2[O:12][C:11]([CH3:15])([CH3:14])[CH2:10][C:9]=2[CH:8]=[CH:7][CH:6]=1.[S:17](Cl)Cl.C(N([CH2:25][CH3:26])CC)C.[NH:27]([CH2:32][C:33]([O:35][CH2:36][CH3:37])=[O:34])[CH2:28][C:29]([O-:31])=[O:30]>C(Cl)(Cl)Cl>[CH2:36]([O:35][C:33]([CH2:32][N:27]([CH2:28][C:29]([O:31][CH2:25][CH3:26])=[O:30])[S:17][N:2]([CH3:1])[C:3](=[O:16])[O:4][C:5]1[C:13]2[O:12][C:11]([CH3:14])([CH3:15])[CH2:10][C:9]=2[CH:8]=[CH:7][CH:6]=1)=[O:34])[CH3:37]

참가 물질

6

반응물 4

HCID 2566CarbofuranHCID 8471Triethylamine2회HCID 25353Sulfur dichlorideHCID 18321666Ethyl iminodiacetate

생성물 1

HCID 3067956Glycine, N-(((((2,3-dihydro-2,2-dimethyl-7-benzofuranyl)oxy)carbonyl)methylamino)thio)-N-(2-ethoxy-2-oxoethyl)-, ethyl ester

시약·촉매·용매 1

HCID 6212Chloroform용매3회

실험 절차

A 11 g quantity (0.05 mole) of 2,3-dihydro-2,2-dimethylbenzofuran-7-yl N-methyl-carbamate was dissolved in 50 ml of chloroform, 5.2 g (0.05 mole) of sulfur dichloride was added to the solution with cooling, and 5 g (0.05 mole) of triethylamine was further added dropwise to the solution at 0° C. The mixture was stirred at the same temperature for 2 hours, a solution of 9.5 g (0.05 mole) of ethyl iminodiacetate in 20 ml of chloroform was then added dropwise to the mixture at the same temperature, and 5 g (0.05 mole) of triethylamine was further added dropwise to the mixture. The resulting mixture was stirred at 0° C. for 2 hours and thereafter allowed to stand overnight at room temperature. With addition of 100 ml of chloroform, the reaction mixture was washed with 100 ml of water three times. The chloroform layer was dried and then concentrated in a vacuum to give an oily product, which was almost entirely composed of the desired product although containing small amounts of the starting materials. Yield: 15.9 g (72.3%).

후처리

  1. temperaturewith cooling
  2. additionwas further added dropwise to the mixture
  3. stirringThe resulting mixture was stirred at 0° C. for 2 hours
  4. waitto stand overnight at room temperature
  5. washthe reaction mixture was washed with 100 ml of water three times
  6. dry with materialThe chloroform layer was dried
  7. concentrationconcentrated in a vacuum
  8. customto give an oily product, which

출처 및 근거

ORD 기록
ord-9e5d27a709114dab95248d07b91ab153
출처 데이터셋
uspto-grants-1983_11
특허 번호
US04413005

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