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

HRID 465287

반응식

HRID 465287 반응식
[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]

참가 물질

5

반응물 3

HCID 1118Sulfuric AcidHCID 5923633-Butene-1,2,3-tricarboxylic acidHCID 178418395HCID 178418395, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c914d1a1f2b646759ac84fa4e23072eb
출처 데이터셋
uspto-grants-1992_10
특허 번호
US05152929

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