Dichloromethane → HCID 178485170, 화합물

HRID 1284963노트

반응식

HRID 1284963 반응식
[OH-].[Na+].S(O)(O)(=O)=O.[CH3:8][NH:9][C:10]([NH2:12])=[NH:11].[O-]S([O-])(=O)=O.[Na+].[Na+].[CH3:20][C:21]1[CH:26]=[C:25]([O:27][CH3:28])[CH:24]=[C:23]([CH3:29])[C:22]=1[N:30]=[C:31]=[O:32].C(Cl)[Cl:34]>C1COCC1.O.Cl.CO>[ClH:34].[CH3:29][C:23]1[CH:24]=[C:25]([O:27][CH3:28])[CH:26]=[C:21]([CH3:20])[C:22]=1[NH:30][C:31]([NH:12][C:10](=[NH:11])[NH:9][CH3:8])=[O:32]

참가 물질

9

반응물 5

HCID 6344DichloromethaneHCID 14798Sodium HydroxideHCID 24436Sodium SulfateHCID 20250931HCID 20250931, 화합물HCID 178485188HCID 178485188, 화합물

생성물 1

HCID 178485170HCID 178485170, 화합물

시약·촉매·용매 3

HCID 962Water용매HCID 8028Tetrahydrofuran용매2회HCID 21893726Hydrochloride methanol용매

실험 절차

7.22 grams of a 50% aqueous sodium hydroxide solution are added to a stirred mixture of methyl guanidine sulfate (9.76 g) in 200 ml of THF. The mixture is stirred for one half hour followed by the addition of anhydrous Na2SO4 (10 g). The mixture is stirred for an additional one half hour. 8.0 grams of 2,6-dimethyl-4-methoxyphenyl isocyanate in 50 ml of THF are added dropwise to the reaction mixture and the mixture stirred overnight. The reaction mixture is filtered and concentrated in vacuo to obtain a yellow oil. The yellow oil is taken up in methylene chloride and water. The methylene chloride layer is dried, filtered and concentrated in vacuo leaving an off-white solid which is dissolved in HCl-methanol, filtered and concentrated in vacuo to a yellow oil which is dissolved in ethyl acetate and methanol and recrystallized to give 7.53 grams of a white solid, M.P. 221°-224° C.

후처리

  1. stirringThe mixture is stirred for an additional one half hour
  2. stirringthe mixture stirred overnight
  3. filtrationThe reaction mixture is filtered
  4. concentrationconcentrated in vacuo
  5. customto obtain a yellow oil
  6. dry with materialThe methylene chloride layer is dried
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo
  9. customleaving an off-white solid which
  10. filtrationfiltered
  11. concentrationconcentrated in vacuo to a yellow oil which
  12. dissolutionis dissolved in ethyl acetate
  13. custommethanol and recrystallized

출처 및 근거

ORD 기록
ord-101a335bbed84172884b5d75f83ce850
출처 데이터셋
uspto-grants-1986_01
특허 번호
US04564640

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