Sulfuric Acid → 4-(Benzothiazol-2-ylthio)-butane-1,2,3-tricarboxylic acid

HRID 465287

反応式

HRID 465287 の反応式
[SH:1][C:2]1[S:3][C:4]2[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=2[N:6]=1.[CH2:11]([C:21]([OH:23])=[O:22])[CH:12]([C:18]([OH:20])=[O:19])[C:13]([C:15]([OH:17])=[O:16])=[CH2:14].OS(O)(=O)=O>O>[S:3]1[C:4]2[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=2[N:6]=[C:2]1[S:1][CH2:14][CH:13]([C:15]([OH:17])=[O:16])[CH:12]([C:18]([OH:20])=[O:19])[CH2:11][C:21]([OH:23])=[O:22]

参加物

5

反応物 3

HCID 1118Sulfuric AcidHCID 5923633-Butene-1,2,3-tricarboxylic acidHCID 178418395HCID 178418395、化合物

生成物 1

HCID 194275694-(Benzothiazol-2-ylthio)-butane-1,2,3-tricarboxylic acid

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

4.45 g of 2-mercaptobenzthiazole, and 5 g of but-3-ene-1,2,3-tricarboxylic acid are ground with one another in a mortar. The powdered mixture is introduced in portions and with stirring into 60 ml of 70% H2SO4 at 48°-50°, in the course of one hour. After a further 3 hours at 48°-50°, the reaction mixture is cooled to room temperature and diluted with 250 ml of water at 25°-30°, with stirring. The aqueous solution is decanted from a little tacky deposit and is diluted with a further 200 ml of water. After being stirred for 1 hour the precipitate is filtered off and dried. The 4-(benzthiazol-2-ylthio)-butane-1,2,3-tricarboxylic acid obtained melts at 188°-190° after recrystallisation from methanol/water.

後処理

  1. additionThe powdered mixture is introduced in portions
  2. customThe aqueous solution is decanted from a little tacky deposit
  3. additionis diluted with a further 200 ml of water
  4. stirringAfter being stirred for 1 hour the precipitate
  5. filtrationis filtered off
  6. customdried

出典と根拠

ORDレコード
ord-c914d1a1f2b646759ac84fa4e23072eb
出典データセット
uspto-grants-1992_10
特許番号
US05152929

関連ノート

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