Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2-Amino-2-methylpropionitrile | HCID 88022 | — |
| Reactant | 71350-98-6 | HCID 12541460 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 13799781 | HCID 13799781 | 133.2% |
Reaction Steps
To a stirred solution of 5.00 g (24.2 mmoles) 2-(methylsulfonyl)ethylsulfonyl chloride (Example 32) in 50 ml dry tetrahydrofuran, a solution of 2.11 g (0.025 moles) 2-amino-2-methyl-propionitrile and 2.5 g (0.025 moles) triethylamine in 20 ml dry tetrahydrofuran were added dropwise over 13 minutes. During the course of the addition, the temperature of the mixture rose from 19° C. to 38° C. and a white precipitate formed. After the mixture cooled to room temperature, it was filtered. The solid, inorganic salts, was washed with tetrahydrofuran and ethyl ether. The filtrate and washings were stripped using a rotovap to give 8.2 g of a sticky white solid. Recrystallization of the solid from boiling ethanol gave 3.94 g of the above-identified product, melting point 151°-153° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04652556 |
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| Source dataset | uspto-grants-1987_03 |
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| ORD ID | ord-6dee50684de44b7e84ad6d3dbed63016 |
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| Source note | uspto-grants-1987_03 |
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