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

HRID 127771

반응식

HRID 127771 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7a9da052dcdf45dbb864d6811b5e88e1
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04256878

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