2-Methyl-2-thiopseudourea sulfate → HCID 13457210, 화합물

HRID 2290321노트

반응식

HRID 2290321 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH:8]1[C:13]([C:14]([O:16][CH3:17])=[O:15])=[C:12]([CH3:18])[NH:11][C:10]([CH2:19][O:20][CH2:21][C:22]([NH:24][NH2:25])=O)=[C:9]1[C:26]([O:28][CH2:29][CH3:30])=[O:27].S(O)(O)(=O)=O.CS[C:38](=[NH:40])[NH2:39].N12CCCC1=NCCC2>C(O)CCC>[NH2:40][C:38]1[N:39]=[C:22]([CH2:21][O:20][CH2:19][C:10]2[NH:11][C:12]([CH3:18])=[C:13]([C:14]([O:16][CH3:17])=[O:15])[CH:8]([C:3]3[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=3[Cl:1])[C:9]=2[C:26]([O:28][CH2:29][CH3:30])=[O:27])[NH:24][N:25]=1

참가 물질

5

반응물 3

HCID 752702-Methyl-2-thiopseudourea sulfateHCID 763491,5-Diazabicyclo(4.3.0)non-5-eneHCID 70044597HCID 70044597, 화합물

생성물 1

HCID 13457210HCID 13457210, 화합물수율 15.3%

시약·촉매·용매 1

HCID 2631-Butanol용매

실험 절차

A solution of 2-{[4-(2-chlorophenyl)-3-ethoxycarbonyl-5-methoxycarbonyl-6-methyl-1,4-dihydropyridin-2-yl]methoxy}-acetylhydrazine (0.87 g), 2-methylisothiourea sulphate (0.68 g) and 1,5-diazabicyclo[4.3.0]non-5-ene (0.74 g) in n-butanol (30 ml) was heated under reflux for 16 hours and then evaporated. The residue was partitioned between dichloromethane and water and the organic layer dried (Na2SO4) and evaporated. The residual oil was purified by chromatography on silica (t.l.c. grade, 10 g) using dichloromethane plus 0-100% v/v ethyl acetate as eluant. Appropriate fractions were combined and evaporated and the residual oil triturated with ethyl acetate. The resulting solid was collected, washed with ethyl acetate and dried to give the title compound (0.14 g), m.p. 199°-202° C. decomp.

후처리

  1. temperatureunder reflux for 16 hours
  2. customevaporated
  3. customThe residue was partitioned between dichloromethane and water
  4. dry with materialthe organic layer dried (Na2SO4)
  5. customevaporated
  6. customThe residual oil was purified by chromatography on silica (t.l.c. grade, 10 g)
  7. customevaporated
  8. customthe residual oil triturated with ethyl acetate
  9. customThe resulting solid was collected
  10. washwashed with ethyl acetate
  11. customdried

출처 및 근거

ORD 기록
ord-cd84fbe6218545f09419eaf47065d42b
출처 데이터셋
uspto-grants-1986_10
특허 번호
US04616024

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