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

HRID 328328

反応式

HRID 328328 の反応式
[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

参加物

7

反応物 5

HCID 76192-(4-Morpholino)thiobenzothiazoleHCID 10340Sodium CarbonateHCID 14798Sodium HydroxideHCID 516892Sodium BicarbonateHCID 23665760Sodium Hypochlorite2 回

生成物 1

HCID 6678152-Morpholinosulphinyl-benzothiazole収率 93%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
25 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-0dd844f0b9774f239f62927bf6b30e8c
出典データセット
uspto-grants-1977_04
特許番号
US04017506

関連ノート

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