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Aluminum(III) Chloride → N-(5-Sulfanyl-1,3-thiazol-2-yl)methanesulfonamide

HRID 127110
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HRID 127110 반응식
[Cl-].[Al+3].[Cl-].[Cl-].[CH3:5][S:6]([NH:9][C:10]1[S:11][C:12]([S:15]CC2C=CC=CC=2)=[CH:13][N:14]=1)(=[O:8])=[O:7]>C1(C)C=CC=CC=1>[CH3:5][S:6]([NH:9][C:10]1[S:11][C:12]([SH:15])=[CH:13][N:14]=1)(=[O:7])=[O:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6451240Aluminum(III) ChlorideHCID 202886432-Methanesulfonamido-5-benzylthiothiazole

생성물 1

HCID 20288660N-(5-Sulfanyl-1,3-thiazol-2-yl)methanesulfonamide수율 30.6%

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

To a mixture of aluminum chloride (510 mg.) and dried toluene (15 ml.) was added 2-methanesulfonamido-5-benzylthiothiazole (560 mg.) over 5 minutes at 110° C. with stirring, and the mixture was further stirred for 1 hour at the same temperature. After the reaction, toluene was removed by decantation. To the residue was added a mixture of water (20 ml.) and methylene chloride (20 ml), and the mixture was stirred for 30 minutes. Thus obtained insoluble material was collected by filtration, washed with water and then dried to give 2-methanesulfonamidothiazole-5-thiol (120 mg.), mp 185° to 192° C. (dec.).

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후처리

  1. stirringthe mixture was further stirred for 1 hour at the same temperature
  2. customwas removed by decantation
  3. additionTo the residue was added
  4. additiona mixture of water (20 ml.) and methylene chloride (20 ml)
  5. stirringthe mixture was stirred for 30 minutes
  6. filtrationThus obtained insoluble material was collected by filtration
  7. washwashed with water
  8. customdried

출처 및 근거

ORD 기록
ord-6db32b5dbe104d3f9a3e8140f39be55a
출처 데이터셋
uspto-grants-1981_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04254260

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