Phosphine, triphenyl-, hydrobromide → (2,4-Dimethyl-5-methoxy-3-thenyl)triphenylphosphonium bromide

HRID 127771

反応式

HRID 127771 の反応式
[CH3:1][C:2]1[S:3][C:4]([O:10][CH3:11])=[C:5]([CH3:9])[C:6]=1[CH2:7]O.[Br-:12].[C:13]1([PH+:19]([C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1>C(#N)C>[Br-:12].[CH3:1][C:2]1[S:3][C:4]([O:10][CH3:11])=[C:5]([CH3:9])[C:6]=1[CH2:7][P+:19]([C:20]1[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=1)([C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)[C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1

参加物

4

反応物 2

HCID 517696Phosphine, triphenyl-, hydrobromideHCID 128752682,4-Dimethyl-3-hydroxymethyl-5-methoxythiophene

生成物 1

HCID 86735242(2,4-Dimethyl-5-methoxy-3-thenyl)triphenylphosphonium bromide

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

6.1 G. (35.5 mmol) of 2,4-dimethyl-3-hydroxymethyl-5-methoxythiophene were added at 35° C. with vigorous stirring to a suspension of 13.4 g. (39.0 mmol) of triphenylphosphonium bromide in 250 ml. of acetonitrile. The deep purple color which was formed immediately, disappeared after some minutes. The reaction mixture was stirred for 3 hrs. The solvent was evaporated to a volume of about 25 ml. and an excess of cold ether was added. The solvent then was decanted from the resulting oily precipitate which was dissolved in warm acetone and again precipitated by adding cold ether. The solvent was decanted and the resulting oily residue was dried in high vacuum to yield (2,4-dimethyl-5-methoxy-3-thenyl)triphenylphosphonium bromide.

後処理

  1. customThe deep purple color which was formed immediately
  2. waitdisappeared after some minutes
  3. stirringThe reaction mixture was stirred for 3 hrs
  4. customThe solvent was evaporated to a volume of about 25 ml
  5. additionand an excess of cold ether was added
  6. customThe solvent then was decanted from the resulting oily precipitate which
  7. dissolutionwas dissolved in warm acetone
  8. customagain precipitated
  9. additionby adding cold ether
  10. customThe solvent was decanted
  11. customthe resulting oily residue was dried in high vacuum

出典と根拠

ORDレコード
ord-7a9da052dcdf45dbb864d6811b5e88e1
出典データセット
uspto-grants-1981_03
特許番号
US04256878

関連ノート

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