반응 #1476309

반응 방정식

hydrochloric acid

Glyoxylic acid hydrate

ammonia

2-Cyclopropylmethyl pyrrole

→

2-(5-Cyclopropylmethyl-2-pyrrolyl)glycine

용매

Diethyl ether

반응 조건

후처리

1. 1
   여과Filtration
2. 2
   기타gave a solid which
3. 3
   세척was washed with diethyl ether (50 ml.)
4. 4
   workup.STIRRINGThe filtrate was shaken
5. 5
   기타the aqueous phase separated
6. 6
   기타to give a slurry whose pH
7. 7
   여과The mixture was filtered
8. 8
   세척the resulting solid thoroughly washed with water, acetone
9. 9
   기타with diethyl ether, affording
10. 10
    건조after drying in vacuo, DL-2-(5-cyclopropylmethyl-2-pyrrolyl)glycine (9.65 g., 55%), M.P. 203°-205° (decomp.)

실험 절차

Glyoxylic acid hydrate (8.3 g., 0.09 mole) was dissolved in 0.880 sp. gr. ammonia solution (50 ml.) and the solution heated to 50°-60°. 2-Cyclopropylmethyl pyrrole (10.9 g., 0.09 mole) was added dropwise and the resulting mixture stirred at 50°-60° for 2 hours. Diethyl ether (50 ml.) was added to the cool reaction mixture. Filtration gave a solid which was washed with diethyl ether (50 ml.). The filtrate was shaken and the aqueous phase separated and combined with the filtered solid to give a slurry whose pH was adjusted to ca. 5 with concentrated hydrochloric acid. The mixture was filtered and the resulting solid thoroughly washed with water, acetone, and with diethyl ether, affording, after drying in vacuo, DL-2-(5-cyclopropylmethyl-2-pyrrolyl)glycine (9.65 g., 55%), M.P. 203°-205° (decomp.).

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