Ethyl (((trifluoromethyl)sulfonyl)oxy)acetate → 3-Ethoxycarbonylmethyl-2-methylbenzotellurazolium Trifluoromethanesulfonate

HRID 622847

반응식

HRID 622847 반응식
[CH3:1][C:2]1[Te:3][C:4]2[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=2[N:6]=1.[F:11][C:12]([F:24])([F:23])[S:13]([O:16][CH2:17][C:18]([O:20][CH2:21][CH3:22])=[O:19])(=[O:15])=[O:14].[Te]1C2C=CC=CC=2N=C1>ClCCl.C(Cl)(Cl)(Cl)Cl>[F:11][C:12]([F:24])([F:23])[S:13]([O-:16])(=[O:15])=[O:14].[CH2:21]([O:20][C:18]([CH2:17][N+:6]1[C:5]2[CH:7]=[CH:8][CH:9]=[CH:10][C:4]=2[Te:3][C:2]=1[CH3:1])=[O:19])[CH3:22]

참가 물질

6

반응물 3

HCID 371745Ethyl (((trifluoromethyl)sulfonyl)oxy)acetateHCID 132147951,3-BenzotellurazoleHCID 132147962-Methyl-1,3-benzotellurazole

생성물 1

HCID 139312343-Ethoxycarbonylmethyl-2-methylbenzotellurazolium Trifluoromethanesulfonate

시약·촉매·용매 2

HCID 5943Carbon Tetrachloride용매HCID 6344Dichloromethane용매

실험 절차

2-Methylbenzotellurazole (Example 18) (0.81 g, 0.0033 mole) was dissolved in dichloromethane (30 ml). The solution of ethoxycarbonylmethyl trifluoromethanesulfonate (0.004 mole) in carbon tetrachloride prepared as described above, was placed in a dropping funnel and added to the benzotellurazole solution at room temperature under a nitrogen atmosphere. After the addition was complete, the mixture was stirred at room temperature, while maintaining a nitrogen atmosphere for 22 hours. The solid was isolated by filtration and dried at room temperature under vacuum. Yield was 0.62 g (39% of theory) of a white powder, m.p. 156°-158° C. The C, H, N and S elemental analyses and the infrared, nuclear magnetic resonance, and mass spectra were all in agreement with that expected for the structural formula.

후처리

  1. customwas placed in a dropping funnel
  2. additionAfter the addition
  3. temperaturewhile maintaining a nitrogen atmosphere for 22 hours
  4. customThe solid was isolated by filtration
  5. customdried at room temperature under vacuum

출처 및 근거

ORD 기록
ord-3abd1d49cfd44e4a86ffad7063528594
출처 데이터셋
uspto-grants-1988_09
특허 번호
US04772715

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