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

HRID 1029354

반응식

HRID 1029354 반응식
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

참가 물질

5

반응물 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

생성물 1

HCID 6457465-Chloro-2-(methylthio)benzothiazole

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-3c95269e58ae498b8021c76427471d47
출처 데이터셋
uspto-grants-1992_04
특허 번호
US05102781

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