반응 #452401

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diphenylphosphine

diphenyl-phosphine

2,2'-azobis (2-methylpropionitrile)

N-vinyl-N-methyl acetamide

→

N-methyl-N-(2-diphenylphosphinoethyl) acetamide

수율 94.0%

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후처리

1. 1
   온도The reaction was maintained at 100° C. for 45 minutes under a nitrogen atmosphere
2. 2
   기타evacuated (1 mm) for 24 hours at 100° C
3. 3
   기타A viscuous oil resulted whose infrared spectrum

실험 절차

A 100 ml 3-necked round bottomed flask was heated to 100° C. under a nitrogen atmosphere and 7.14 g diphenyl-phosphine (38.4 mmole), 0.15 g 2,2'-azobis (2-methylpropionitrile), and 3.77 g N-vinyl-N-methyl acetamide (38.1 mmole) from Polysciences were added in the stated sequence. The reaction was maintained at 100° C. for 45 minutes under a nitrogen atmosphere and then evacuated (1 mm) for 24 hours at 100° C. A viscuous oil resulted whose infrared spectrum displayed a strong γ (CO) band at 1645 cm-1 and a small γ (P-H) band at 2300 cm-1 due to a small amount of diphenylphosphine impurity. The elemental analysis was the following: calculated (found); C, 71.58 (69.89); H, 7.02 (7.15); N, 4.91 (4.57); P, 10.87 (10.97). The yield was 94%.

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