Potassium Carbonate → N-(4-Ethoxycarbonylamino-1-methyl-5-pyrazolesulfonyl)-N'-isopropylthiourea

HRID 1419761노트

반응식

HRID 1419761 반응식
[CH3:1][N:2]1[C:6]([S:7]([NH2:10])(=[O:9])=[O:8])=[C:5]([NH:11][C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH:4]=[N:3]1.C(=O)([O-])[O-].[K+].[K+].[CH:23]([N:26]=[C:27]=[S:28])([CH3:25])[CH3:24]>CC(C)=O>[CH2:15]([O:14][C:12]([NH:11][C:5]1[CH:4]=[N:3][N:2]([CH3:1])[C:6]=1[S:7]([NH:10][C:27]([NH:26][CH:23]([CH3:25])[CH3:24])=[S:28])(=[O:9])=[O:8])=[O:13])[CH3:16]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 75263Isopropyl IsothiocyanateHCID 540732311-Methyl-4-(ethoxycarbonylamino)pyrazole-5-sulfonamide

생성물 1

HCID 54068939N-(4-Ethoxycarbonylamino-1-methyl-5-pyrazolesulfonyl)-N'-isopropylthiourea수율 64%

시약·촉매·용매 1

HCID 180Acetone용매

반응 조건

온도
55 °C

실험 절차

A mixture of 1-methyl-4-(ethoxycarbonylamino)pyrazole-5-sulfonamide (0.42 g), potassium carbonate (0.34 g) and isopropyl isothiocyanate (280 μl) in 10 ml of dry acetone was heated at 55° C. for 18 h and then evaporated to dryness. The residue was dissolved in 10 ml of water, and pH was adjusted to 2 by dropwise addition of 4M hydrochloric acid. The precipitate was filtered off, rinsed with a small amount of water and dried to give 0.38 g (64%) of the title compound; m.p. 141°-144° C.

후처리

  1. customevaporated to dryness
  2. dissolutionThe residue was dissolved in 10 ml of water
  3. additionpH was adjusted to 2 by dropwise addition of 4M hydrochloric acid
  4. filtrationThe precipitate was filtered off
  5. washrinsed with a small amount of water
  6. customdried

출처 및 근거

ORD 기록
ord-c24657c2066e441990f223686538985d
출처 데이터셋
uspto-grants-1999_03
특허 번호
US05889002

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