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

HRID 224350ノート

反応式

HRID 224350 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3820fdd409ce450eaa003f1788cb2acb
出典データセット
uspto-grants-1980_11
特許番号
US04232024

反応ノート

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