2-(4-Morpholino)thiobenzothiazole → 2-Morpholinosulphinyl-benzothiazole

HRID 328328

반응식

HRID 328328 반응식
[O:1]1[CH2:6][CH2:5][N:4]([S:7][C:8]2[S:9][C:10]3[CH:16]=[CH:15][CH:14]=[CH:13][C:11]=3[N:12]=2)[CH2:3][CH2:2]1.C(=O)([O-])[O-:18].[Na+].[Na+].C(=O)(O)[O-].[Na+].Cl[O-].[Na+].[OH-].[Na+]>O>[O:1]1[CH2:6][CH2:5][N:4]([S:7]([C:8]2[S:9][C:10]3[CH:16]=[CH:15][CH:14]=[CH:13][C:11]=3[N:12]=2)=[O:18])[CH2:3][CH2:2]1

참가 물질

7

반응물 5

HCID 76192-(4-Morpholino)thiobenzothiazoleHCID 10340Sodium CarbonateHCID 14798Sodium HydroxideHCID 516892Sodium BicarbonateHCID 23665760Sodium Hypochlorite2회

생성물 1

HCID 6678152-Morpholinosulphinyl-benzothiazole수율 93%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
25 °C

실험 절차

37.8 parts of 2-morpholinosulphenyl-benzothiazole are suspended in 65 parts of water containing 5 parts of sodium carbonate and 1 part of sodium bicarbonate. 90 parts by volume of an aqueous solution of sodium hypochlorite titrating 177 g. of NaClO and 3 g. of free caustic soda per liter are slowly introduced in a period of one hour into the well stirred suspension. The temperature is maintained at 25° C. and the mixture is stirred for 20 hours at this temperature. It is filtered, the solid is washed until neutral and dried under vacuum. 37 parts of 2-morpholinosulphinyl-benzothiazole melting at 93°-94° C. are obtained, that is a yield of 93%. On recrystallisation from a benzene/petrol ether mixture, the melting point is 99° C. (uncorrected).

후처리

  1. stirringthe mixture is stirred for 20 hours at this temperature
  2. filtrationIt is filtered
  3. washthe solid is washed until neutral and
  4. customdried under vacuum

출처 및 근거

ORD 기록
ord-0dd844f0b9774f239f62927bf6b30e8c
출처 데이터셋
uspto-grants-1977_04
특허 번호
US04017506

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