Triethylamine → N-[6-(n-butyl)-4H-1-benzothiopyran-4-on-3-yl]-oxalic acid amide methyl ester

HRID 65467노트

반응식

HRID 65467 반응식
[Cl-].[CH3:2][O:3][C:4](=[O:8])[C:5]([OH:7])=O.[NH2:9][C:10]1[C:15](=[O:16])[C:14]2[CH:17]=[C:18]([CH2:21][CH2:22][CH2:23][CH3:24])[CH:19]=[CH:20][C:13]=2[S:12][CH:11]=1.C(N(CC)CC)C>C(Cl)(Cl)Cl>[CH3:2][O:3][C:4](=[O:8])[C:5]([NH:9][C:10]1[C:15](=[O:16])[C:14]2[CH:17]=[C:18]([CH2:21][CH2:22][CH2:23][CH3:24])[CH:19]=[CH:20][C:13]=2[S:12][CH:11]=1)=[O:7]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 202331283-amino-6-(n-butyl)-4H-1-benzothiopyran-4-oneHCID 86640482Oxalic acid monomethyl ester chloride

생성물 1

HCID 86741042N-[6-(n-butyl)-4H-1-benzothiopyran-4-on-3-yl]-oxalic acid amide methyl ester

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

2.94 g (0.024 mol) of oxalic acid monomethyl ester chloride are added to a solution of 5.05 g (0.0216 mol) of 3-amino-6-(n-butyl)-4H-1-benzothiopyran-4-one and 2.4 g (0.024 mol) of triethylamine in 325 ml of chloroform, the temperature of the reaction mixture rising to 30°. The mixture is then stirred for one hour at room temperature. The mixture is then concentrated to dryness by evaporation and the crystalline residue is stirred with ethanol, filtered with suction and washed first with ethanol and then with ether. After drying, N-[6-(n-butyl)-4H-1-benzothiopyran-4-on-3-yl]-oxalic acid amide methyl ester having a melting point of 192°-193.5° is obtained.

후처리

  1. customrising to 30°
  2. concentrationThe mixture is then concentrated to dryness by evaporation
  3. stirringthe crystalline residue is stirred with ethanol
  4. filtrationfiltered with suction
  5. washwashed first with ethanol
  6. customAfter drying

출처 및 근거

ORD 기록
ord-8f68ced42d6240b895461757e3233495
출처 데이터셋
uspto-grants-1986_09
특허 번호
US04614745

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