Ethyl chloroformate → HCID 19023425, compound

HRID 2082145Notes

Reaction equation

HRID 2082145 reaction equation
[N:1]1[CH:6]=[CH:5][CH:4]=[N:3][C:2]=1[N:7]1[CH2:12][CH2:11][N:10]([CH2:13][CH2:14][CH2:15][CH2:16][N:17]2[C:21](=[O:22])[C:20]3[CH:23]=[CH:24][C:25]([NH2:27])=[CH:26][C:19]=3[S:18]2(=[O:29])=[O:28])[CH2:9][CH2:8]1.Cl[C:31]([O:33][CH2:34][CH3:35])=[O:32]>N1C=CC=CC=1>[N:3]1[CH:4]=[CH:5][CH:6]=[N:1][C:2]=1[N:7]1[CH2:12][CH2:11][N:10]([CH2:13][CH2:14][CH2:15][CH2:16][N:17]2[C:21](=[O:22])[C:20]3[CH:23]=[CH:24][C:25]([NH:27][C:31]([O:33][CH2:34][CH3:35])=[O:32])=[CH:26][C:19]=3[S:18]2(=[O:28])=[O:29])[CH2:9][CH2:8]1

Participants

4

Reactant 2

HCID 10928Ethyl chloroformateHCID 19023477HCID 19023477, compound

Product 1

HCID 19023425HCID 19023425, compound

Reagents, catalysts & solvents 1

HCID 1049PyridineSolvent

Procedure

0.01 mol of 2-(4-(4-(2-pyrimidinyl)-1-piperazinyl)butyl)-6-amino-1,2-benzisothiazol-3(2H)one 1,1-dioxide is dissolved in 30 ml of absolute pyridine and, via cooling in ice, 0.02 mol of ethyl chloroformate is added. The mixture is then allowed to reach room temperature and is stirred for 12 hours. The solvent is evaporated off, ice-water is added and the mixture is extracted by shaking several times with methylene chloride. Colourless crystals are obtained after evaporating off the solvent.

Workup

  1. temperaturevia cooling in ice
  2. customto reach room temperature
  3. customThe solvent is evaporated off
  4. additionice-water is added
  5. extractionthe mixture is extracted
  6. stirringby shaking several times with methylene chloride
  7. customColourless crystals are obtained
  8. customafter evaporating off the solvent

Sources & evidence

ORD record
ord-51fffb1704434f30b352c010f5d63dde
Source dataset
uspto-grants-1993_02
Patent number
US05187276

Reaction notes

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