Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Isobutyl chloroformate | HCID 62365 | — |
| Reactant | HCID 19001522 | HCID 19001522 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 19001536 | HCID 19001536 | — |
Reaction Steps
90 g of the N-(6-nitrobenzothiazol-2-yl)isonipecotic acid obtained in the Preparation Example 11 was suspended in 500 ml of tetrahydrofuran and 1,000 ml of dimethylformamide. 100 ml of triethylamine was added to the suspension and 45 ml of isobutyl chlorocarbonate was added dropwise to the suspension under cooling to -20° C. After stirring for 20 min, 100 ml of concentrated aqueous ammonia was added to the mixture at -40° C. and stirred for 20 min. The reaction mixture was poured into ice/water and the formed precipitates were recovered by filtration, washed with water and then with ether, and dried to give 75 g of the titled compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05475014 |
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| Source dataset | uspto-grants-1995_12 |
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| ORD ID | ord-daf0d2cb7a8749c497599f835dbf98aa |
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| Source note | uspto-grants-1995_12 |
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