Carbamic acid, (1,3-dioxo-1,3-propanediyl)bis-, diethyl ester → HCID 11329229, 화합물

HRID 1072477

반응식

HRID 1072477 반응식
[N:1]([O-])=O.[Na+].[NH2:5][C:6]1[CH:11]=[C:10]([Cl:12])[C:9]([C:13]([CH3:17])([CH3:16])[C:14]#[N:15])=[C:8]([Cl:18])[CH:7]=1.C([O-])(=O)C.[Na+].[CH2:24]([O:26][C:27](=[O:40])[NH:28][C:29](=[O:39])[CH2:30][C:31]([NH:33][C:34](=[O:38])[O:35][CH2:36][CH3:37])=[O:32])[CH3:25]>O.C(O)(=O)C.Cl>[Cl:18][C:8]1[CH:7]=[C:6]([NH:5][N:1]=[C:30]([C:31]([NH:33][C:34](=[O:38])[O:35][CH2:36][CH3:37])=[O:32])[C:29]([NH:28][C:27](=[O:40])[O:26][CH2:24][CH3:25])=[O:39])[CH:11]=[C:10]([Cl:12])[C:9]=1[C:13]([C:14]#[N:15])([CH3:16])[CH3:17]

참가 물질

8

반응물 4

HCID 154305Carbamic acid, (1,3-dioxo-1,3-propanediyl)bis-, diethyl esterHCID 517045Sodium AcetateHCID 112416692-(4-Amino-2,6-dichloro-phenyl)-2-methyl-propionitrileHCID 23668193Sodium Nitrite

생성물 1

HCID 11329229HCID 11329229, 화합물수율 84%

시약·촉매·용매 3

HCID 176Acetic Acid용매HCID 313Hydrochloric Acid용매HCID 962Water용매

반응 조건

온도
10 °C

실험 절차

A solution of NaNO2 (0.36 mole) in H2O (50 ml) was added to a solution of intermediate (3) (0.34 mole) in acetic acid (700 ml) and HCl (102 ml), stirred at 10° C. The reaction mixture was stirred for 80 minutes at 10° C. A powdered mixture of sodium acetate (1.02 mole) and diethyl(1,3-dioxo-1,3-propanediyl)biscarbamate (0.374 mole) was added and the reaction mixture was stirred for 40 minutes. The reaction mixture was poured out onto crushed ice. The precipitate was filtered off, washed with water, taken up into CH2Cl2, and the layers were separated. The organic layer was dried, filtered and the solvent evaporated, yielding 138.5 g (84%) of diethyl N,N′-[2-[[3,5-dichloro-4-(1-cyano-1-methylethyl)phenyl]hydrazono]-1,3-dioxo-1,3-propanediyl]dicarbamate (intermediate 4).

후처리

  1. stirringThe reaction mixture was stirred for 80 minutes at 10° C
  2. additionwas added
  3. stirringthe reaction mixture was stirred for 40 minutes
  4. additionThe reaction mixture was poured out
  5. customonto crushed ice
  6. filtrationThe precipitate was filtered off
  7. washwashed with water
  8. customthe layers were separated
  9. customThe organic layer was dried
  10. filtrationfiltered
  11. customthe solvent evaporated

출처 및 근거

ORD 기록
ord-e3baf4461cee4dd18dced4638a922300
출처 데이터셋
uspto-grants-2005_06
특허 번호
US06911444B2

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