Triethylamine → 4-[3-Ethylbenzothiazolinylidene]-3-methyl-1-phenylpyrazolin-5-one

HRID 1029363ノート

反応式

HRID 1029363 の反応式
[CH3:1][C:2]1[NH:3][N:4]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[C:5](=[O:7])[CH:6]=1.S(C1C=CC(C)=CC=1)([O-])(=O)=O.C(S[C:28]1[S:29][C:30]2[CH:38]=[CH:37][CH:36]=[CH:35][C:31]=2[N+:32]=1[CH2:33][CH3:34])C.C(N(CC)CC)C>CO>[CH2:33]([N:32]1[C:31]2[CH:35]=[CH:36][CH:37]=[CH:38][C:30]=2[S:29](=[C:6]2[C:5](=[O:7])[N:4]([C:8]3[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=3)[NH:3][CH:2]2[CH3:1])[CH2:28]1)[CH3:34]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 703351H-Pyrazol-5-ol, 3-methyl-1-phenyl-HCID 140905473-Ethyl-2-(ethylsulfanyl)-1,3-benzothiazol-3-ium 4-methylbenzene-1-sulfonate

生成物 1

HCID 867456164-[3-Ethylbenzothiazolinylidene]-3-methyl-1-phenylpyrazolin-5-one

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

3-Methyl-1-phenylpyrazolin-5-one (1.74 g, 0.01 mol) was mixed with a methanol solution of 2-ethylthio-3-ethylbenzothiazolium tosylate. Triethylamine (1.01 g, 0.01 mol) was added. The mixture was stirred for 10 minutes, then concentrated and treated with isopropanol. The mixture was heated to dissolve the product, then water was added to cloud, and the mixture cooled to give crystals: 3.22 g (48%), mp 144°-147.5° C., λmax=379 (ε=25,000).

後処理

  1. concentrationconcentrated
  2. additiontreated with isopropanol
  3. temperatureThe mixture was heated
  4. dissolutionto dissolve the product
  5. additionwater was added to cloud
  6. temperaturethe mixture cooled
  7. customto give crystals

出典と根拠

ORDレコード
ord-b931c63ecf554f069f4279a9ac934fab
出典データセット
uspto-grants-1992_04
特許番号
US05102781

反応ノート

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