Iodoethane → Ethyl-7-methoxy-1-oxo-1H-pyrimido[6,1-b]benzthiazole-4-carboxylate

HRID 224350노트

반응식

HRID 224350 반응식
[Na].[CH3:2][O:3][C:4]1[CH:20]=[CH:19][C:7]2[N:8]3[C:14](=[O:15])[N:13]=[CH:12][C:11]([C:16]([OH:18])=[O:17])=[C:9]3[S:10][C:6]=2[CH:5]=1.O=P(N(C)C)(N(C)C)N(C)C.[CH2:32](I)[CH3:33]>O>[CH2:32]([O:17][C:16]([C:11]1[CH:12]=[N:13][C:14](=[O:15])[N:8]2[C:7]3[CH:19]=[CH:20][C:4]([O:3][CH3:2])=[CH:5][C:6]=3[S:10][C:9]=12)=[O:18])[CH3:33]

참가 물질

6

반응물 4

HCID 6340IodoethaneHCID 12679HexamethylphosphoramideHCID 5360545SodiumHCID 233327897-Methoxy-1-oxo-1H-pyrimido[6,1-b]benzthiazole-4-carboxylic acid

생성물 1

HCID 23332809Ethyl-7-methoxy-1-oxo-1H-pyrimido[6,1-b]benzthiazole-4-carboxylate

시약·촉매·용매 1

HCID 962Water용매

실험 절차

20 g. of the sodium salt of 7-methoxy-1-oxo-1H-pyrimido[6,1-b]benzthiazole-4-carboxylic acid prepared according to Example 1C are slurried in 200 ml. hexametapol and mixed at ambient temperature with 23.45 g. ethyl iodide. The reaction mixture is stirred for 80 minutes and the resultant solution poured into 3 liters of water. The precipitate obtained is separated off and, while still moist, boiled with 500 ml. ethanol and brought into solution by the addition of some nitromethane. After cooling, 12.9 g. (63.3% of theory) ethyl 7-methoxy-1-oxo-1H-pyrimido[6,1-b]benzthiazole-4-carboxylate crystallize out; m.p. 231°-232° C.

후처리

  1. customThe precipitate obtained
  2. customis separated off
  3. additionethanol and brought into solution by the addition of some nitromethane
  4. temperatureAfter cooling
  5. custom(63.3% of theory) ethyl 7-methoxy-1-oxo-1H-pyrimido[6,1-b]benzthiazole-4-carboxylate crystallize out

출처 및 근거

ORD 기록
ord-3820fdd409ce450eaa003f1788cb2acb
출처 데이터셋
uspto-grants-1980_11
특허 번호
US04232024

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