1,3-Dichloropropane → Phosphine, (3-chloropropyl)diphenyl-

HRID 4761

反応式

HRID 4761 の反応式
[PH:1]([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C([Li])CCC.[Li]P(C1C=CC=CC=1)C1C=CC=CC=1.[Cl:33][CH2:34][CH2:35][CH2:36]Cl>C(OCC)C.O.O1CCCC1>[P:1]([CH2:36][CH2:35][CH2:34][Cl:33])([C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

8

反応物 4

HCID 88811,3-DichloropropaneHCID 70017DiphenylphosphineHCID 178418339ButyllithiumHCID 178418495HCID 178418495、化合物

生成物 1

HCID 608029Phosphine, (3-chloropropyl)diphenyl-

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 3283Diethyl Ether溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

To a 500 mL round bottom flask there was added 400 mL of dry tetrahydrofuran followed by 0.081 mole of HPPh2. The mixture was cooled to 0° C. and 0.081 mole of n-butyl lithium was slowly added to generate LiPPh2 ; this was slowly warmed to room temperature and stirred for about one hour. The solution was transferred to a dropping funnel and added dropwise to a flask containing 100 mL of 1,3-dichloropropane dissolved in 100 mL of diethyl ether. After stirring overnight the mixture was hydrolyzed with 25 mL of water. The organic layer was separated and the solvent removed by vacuum to leave Ph2P(CH2)3Cl that was stored under nitrogen until needed.

後処理

  1. temperaturethis was slowly warmed to room temperature
  2. customThe solution was transferred to a dropping funnel
  3. additionadded dropwise to a flask
  4. stirringAfter stirring overnight the mixture
  5. customThe organic layer was separated
  6. customthe solvent removed by vacuum

出典と根拠

ORDレコード
ord-12421d0797394bc59f5eb474f7a37fd6
出典データセット
uspto-grants-1988_02
特許番号
US04727200

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