Triethylamine → 5-Chloro-2-(methylthio)benzothiazole

HRID 1029354

反応式

HRID 1029354 の反応式
CC1NN(C2C=CC=CC=2)C(=O)C=1.[CH3:14][S:15][C:16]1[S:17][C:18]2[CH:31]=[CH:30][C:29]([Cl:32])=[CH:28][C:19]=2[N+:20]=1CCCS(O)(=O)=O.C(N(CC)CC)C>CO>[Cl:32][C:29]1[CH:30]=[CH:31][C:18]2[S:17][C:16]([S:15][CH3:14])=[N:20][C:19]=2[CH:28]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 703351H-Pyrazol-5-ol, 3-methyl-1-phenyl-HCID 43837363-[5-Chloro-2-(methylthio)-1,3-benzothiazol-3-ium-3-yl]-1-propanesulfonate

生成物 1

HCID 6457465-Chloro-2-(methylthio)benzothiazole

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

3-Methyl-1-phenylpyrazolin-5-one (1.045 g) was mixed with 2.03 g (0.006 mol) 2-methylthio-5-chloro-3-(3'-sulfopropyl)benzothiazolium, inner salt in 50 ml methanol. Triethylamine (0.62 g) was added. The mixture was stirred for one hour, the solvent evaporated, and the residue dissolved in isopropanol. The resulting solution was treated with 0.6 g KOAc in methanol to precipitate the dye. Filtering yielded 2.17 g (72%), mp 271°-276° C., λmax=383 (ε=19,000).

後処理

  1. customthe solvent evaporated
  2. dissolutionthe residue dissolved in isopropanol
  3. additionThe resulting solution was treated with 0.6 g KOAc in methanol
  4. customto precipitate the dye
  5. filtrationFiltering
  6. customyielded 2.17 g (72%), mp 271°-276° C., λmax=383 (ε=19,000)

出典と根拠

ORDレコード
ord-3c95269e58ae498b8021c76427471d47
出典データセット
uspto-grants-1992_04
特許番号
US05102781

関連ノート

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