Trifluoroiodomethane → HCID 13340634、化合物

HRID 1632731ノート

反応式

HRID 1632731 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[N:10]([CH3:22])[CH:11]=[CH:12][C:13]=2[C:14]2[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=2)=[CH:5][CH:4]=1.C(N(C(C)C)C(C)C)C.[F:32][C:33](I)([F:35])[F:34]>>[CH3:21][O:20][C:17]1[CH:18]=[CH:19][C:14]([C:13]2[CH:12]=[C:11]([C:33]([F:35])([F:34])[F:32])[N:10]([CH3:22])[C:9]=2[C:6]2[CH:5]=[CH:4][C:3]([O:2][CH3:1])=[CH:8][CH:7]=2)=[CH:15][CH:16]=1

参加物

4

反応物 3

HCID 16843TrifluoroiodomethaneHCID 81531DiisopropylethylamineHCID 133406332,3-Bis(4-methoxyphenyl)-1-methyl-1H-pyrrole

生成物 1

HCID 13340634HCID 13340634、化合物

実験手順

In a pressure reaction vessel was placed 2.9 g (0.01 mole) of 2,3-bis(4-methoxyphenyl)-1-methyl-1H-pyrrole and 1.3 g (0.01 mole) of ethyl diisopropylamine. The vessel was cooled and evacuated, and 2.0 g (0.01 mole) of trifluoromethyl iodide was added. The mixture was heated at 150° for approximately 18 hours. The vessel was cooled and vented, and the contents rinsed out with methylene chloride. The methylene chloride solution was washed with water three times then dried and concentrated to give the crude product. This was purified by chromatography on 400 g silica gel, eluting with toluene, to give after recrystallization from hexane, 1.0 g (28%) of product as a white solid, m.p. 125°-126°.

後処理

  1. customIn a pressure reaction vessel
  2. temperatureThe vessel was cooled
  3. customevacuated
  4. temperatureThe mixture was heated at 150° for approximately 18 hours
  5. temperatureThe vessel was cooled
  6. washthe contents rinsed out with methylene chloride
  7. washThe methylene chloride solution was washed with water three times
  8. customthen dried
  9. concentrationconcentrated

出典と根拠

ORDレコード
ord-acf88cb7b2f944d5bc6e0ed3b98e8204
出典データセット
uspto-grants-1984_10
特許番号
US04477463

反応ノート

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