Acetic Acid → 2-[[(1-Ethyl-5-methylthio-1H-1,2,4-triazol-3-yl)aminocarbonyl]aminosulfonyl]benzoic acid, methyl ester

HRID 904988노트

반응식

HRID 904988 반응식
[CH3:1][S:2][C:3]1[NH:7][N:6]=[C:5]([NH:8][C:9]([NH:11][S:12]([C:15]2[CH:24]=[CH:23][CH:22]=[CH:21][C:16]=2[C:17]([O:19][CH3:20])=[O:18])(=[O:14])=[O:13])=[O:10])[N:4]=1.C(=O)([O-])[O-].[K+].[K+].[CH2:31](I)[CH3:32].C(O)(=O)C>CC(C)=O.C(#N)C>[CH2:31]([N:7]1[C:3]([S:2][CH3:1])=[N:4][C:5]([NH:8][C:9]([NH:11][S:12]([C:15]2[CH:24]=[CH:23][CH:22]=[CH:21][C:16]=2[C:17]([O:19][CH3:20])=[O:18])(=[O:14])=[O:13])=[O:10])=[N:6]1)[CH3:32]

참가 물질

7

반응물 4

HCID 176Acetic AcidHCID 6340IodoethaneHCID 11430Potassium CarbonateHCID 178497660HCID 178497660, 화합물

생성물 1

HCID 132453552-[[(1-Ethyl-5-methylthio-1H-1,2,4-triazol-3-yl)aminocarbonyl]aminosulfonyl]benzoic acid, methyl ester

시약·촉매·용매 2

HCID 180Acetone용매HCID 6342Acetonitrile용매

실험 절차

To a stirred mixture of 1.0 gram (0.0027 mole) of methyl 2-[(5-methylthio-1H-1,2,4-triazol-3-yl)aminocarbonyl]aminosulfonylbenzoate and 0.7 grams of potassium carbonate in 30 ml of acetone at room temperature, 0.8 ml of ethyl iodine was added by way of syringe and the resulting white suspension stirred 3 days. The mixture was poured into 250 ml of ice water and acidified to pH 3-4 with glacial acetic acid. The aqueous acidic mixture was extracted with 1:1 mixture of ethyl ether/ethyl acetate and the extract washed with brine, dried (MgSO4), and evaporated to yield a white solid residue which was suspended in acetonitrile and filtered, yield 0.3 grams, m.p. 188°-191°.

후처리

  1. extractionThe aqueous acidic mixture was extracted with 1:1 mixture of ethyl ether/ethyl acetate
  2. washthe extract washed with brine
  3. dry with materialdried (MgSO4)
  4. customevaporated
  5. customto yield a white solid residue which
  6. filtrationfiltered

출처 및 근거

ORD 기록
ord-0feed14454cc43edbc49b5a594be27c9
출처 데이터셋
uspto-grants-1983_12
특허 번호
US04421550

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