Acetic Anhydride → HCID 20373177, compound

HRID 1834415Notes

Reaction equation

I.C(O[C:6](=O)[CH3:7])(=O)C.[PH2](O)=O.[CH3:12][C:13]1[NH:14][CH:15]=[C:16]([CH3:21])[C:17]=1[C:18](=[O:20])[CH3:19]>C1(=O)CCCCC1.O>[CH3:12][C:13]1[NH:14][C:15]([CH:7]2[CH2:6][CH2:16][CH2:17][CH2:13][CH2:12]2)=[C:16]([CH3:21])[C:17]=1[C:18](=[O:20])[CH3:19]

Participants

Conditions

Temperature: 40 °C

Procedure

A solution of 10 ml of aqueous hydriodic acid, 10 ml of acetic anhydride and 2 ml of 50% hypophosphorous acid was stirred magnetically at 40° C. while 548 mg of 2,4-dimethyl-3-acetyl-pyrrole were dissolved in it, 0.5 ml of cyclohexanone was then added, and an additional 0.5 ml of cyclohexanone was added after a few minutes'. The solution was stirred at 40° C. for 11/2 hrs. then poured into water. The crude product which separated, m.p. 186°-188° C. was recrystallized from ethanol as colourless rhombic prisms (82%), m.p. 188.5°-189° C. after changing to flat prisms above 153° C.

Workup

additionwas then added
customThe crude product which separated
customm.p. 186°-188° C. was recrystallized from ethanol as colourless rhombic prisms (82%), m.p. 188.5°-189° C.
customafter changing to flat prisms above 153° C.

Sources & evidence

ORD record: ord-a3c275d2ee4141f3a9c1acda8828e7c2
Source dataset: uspto-grants-1978_01
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US04070366

Reaction notes

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