Sodium Acetate → HCID 178481663、化合物

HRID 839475

反応式

HRID 839475 の反応式
[OH-].[CH3:2][N+:3]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[S:5][C:4]=1SCCCS(O)(=O)=O.Cl.Cl.[NH2:22][C:23]1[CH:31]=[CH:30][C:26]2[NH:27][N:28]=[N:29][C:25]=2[CH:24]=1.C([O-])(=O)C.[Na+]>O>[CH3:2][N:3]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[S:5](=[N:22][C:23]2[CH:31]=[CH:30][C:26]3[NH:27][N:28]=[N:29][C:25]=3[CH:24]=2)[CH2:4]1

参加物

5

反応物 3

HCID 517045Sodium AcetateHCID 867357563-Methyl-2-(3-sulfopropylthio) benzothiazolium hydroxideHCID 178478652HCID 178478652、化合物

生成物 1

HCID 178481663HCID 178481663、化合物収率 98.7%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

反応条件

温度
50 °C

実験手順

175 g of anhydrous 3-methyl-2-(3-sulfopropylthio) benzothiazolium hydroxide was added to a mixture of 100 g of 5-aminobenzotriazole di-hydrochloride, 120 g of sodium acetate and 1000 ml of water under heating at 50° C with stirring in a 2000 ml flask. After stirring for 1 hour at 85° C the mixture was cooled (15° C) with water. The precipitate formed was collected by filtration, washed with water and then with acetonitrile to yield 135 g of crystals. These crystals were dissolved by heating (90° C) in 350 ml of dimethylformamide and the solution was treated with active carbon and filtered. By addition of 1400 ml of acetonitrile to the filtrate, crystals were formed. The crystals were collected to yield 121 g of the desired compound. The melting point was 240.5° C.

後処理

  1. stirringAfter stirring for 1 hour at 85° C the mixture
  2. customThe precipitate formed
  3. filtrationwas collected by filtration
  4. washwashed with water

出典と根拠

ORDレコード
ord-83e9387fa1c541aeaaebcb2cb3c4802e
出典データセット
uspto-grants-1978_06
特許番号
US04095984

関連ノート

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