Ethyl chloroformate → HCID 19023425, compound

HRID 620055Notes

Reaction equation

HRID 620055 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-636f8eb6bf22477d96934f244efc39e5
Source dataset
uspto-grants-1989_04
Patent number
US04818756

Reaction notes

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