Phosphine, triphenyl-, hydrobromide → [1-(4,5,6,7-Tetrahydro-4,4,7,7-tetramethylbenzo-[b]thien-2-yl)ethyl]triphenylphosphonium bromide

HRID 1194785노트

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HRID 1194785 반응식
[CH3:1][CH:2]([C:4]1[S:8][C:7]2[C:9]([CH3:16])([CH3:15])[CH2:10][CH2:11][C:12]([CH3:14])([CH3:13])[C:6]=2[CH:5]=1)O.[Br-:17].[C:18]1([PH+:24]([C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)[C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1>C(#N)C>[Br-:17].[CH3:13][C:12]1([CH3:14])[C:6]2[CH:5]=[C:4]([CH:2]([P+:24]([C:25]3[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=3)([C:31]3[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=3)[C:18]3[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=3)[CH3:1])[S:8][C:7]=2[C:9]([CH3:16])([CH3:15])[CH2:10][CH2:11]1

참가 물질

4

반응물 2

HCID 517696Phosphine, triphenyl-, hydrobromideHCID 867402444,5,6,7-Tetrahydro-alpha,4,4,7,7-pentamethylbenzo[b]thiophene-methanol

생성물 1

HCID 23049224[1-(4,5,6,7-Tetrahydro-4,4,7,7-tetramethylbenzo-[b]thien-2-yl)ethyl]triphenylphosphonium bromide수율 103.4%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

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온도
50 °C

실험 절차

20.2 g of 4,5,6,7-tetrahydro-α,4,4,7,7-pentamethylbenzo[b]thiophene-methanol are dissolved in 260 ml of acetonitrile and the solution is treated with 29.2 g of triphenylphosphonium bromide. After stirring at 50° C. for 3 hours, the mixture is evaporated to dryness, the residue is taken up with 80% aqueous ethanol and extracted twice with hexane. The ethanol phase is evaporated, the residue is dissolved in methylene chloride, the solution is dried over sodium sulphate and evaporated. There are obtained 49.4 g of [1-(4,5,6,7-tetrahydro-4,4,7,7-tetramethylbenzo[b]thien-2-yl)ethyl]triphenylphosphonium bromide as an amorphous white powder.

후처리

  1. customthe mixture is evaporated to dryness
  2. extractionextracted twice with hexane
  3. customThe ethanol phase is evaporated
  4. dissolutionthe residue is dissolved in methylene chloride
  5. dry with materialthe solution is dried over sodium sulphate
  6. customevaporated

출처 및 근거

ORD 기록
ord-8a716cf9a7f84464858b1a5c892c753e
출처 데이터셋
uspto-grants-1989_03
특허 번호
US04816476

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