Triphenylphosphine → {3-[(Oxan-2-yl)oxy]propyl}(triphenyl)phosphanium iodide

HRID 652462

反応式

HRID 652462 の反応式
[I:1][CH2:2][CH2:3][CH2:4][O:5][CH:6]1[CH2:11][CH2:10][CH2:9][CH2:8][O:7]1.[C:12]1([P:18]([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1>C1C=CC=CC=1>[I-:1].[O:7]1[CH2:8][CH2:9][CH2:10][CH2:11][CH:6]1[O:5][CH2:4][CH2:3][CH2:2][P+:18]([C:19]1[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1)([C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1)[C:12]1[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=1

参加物

4

反応物 2

HCID 11776TriphenylphosphineHCID 110329072-(3-iodopropoxy)tetrahydro-2H-pyran

生成物 1

HCID 20196785{3-[(Oxan-2-yl)oxy]propyl}(triphenyl)phosphanium iodide

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

A solution of 3-iodo-1-tetrahydro-2-pyranyloxy propane (20.43 g, 75.63 mmole), and triphenylphosphine (19.84 g, 75.63 mmole) in 150 ml of dry benzene was refluxed under an atmosphere of nitrogen for 24 hours. The solvent was evaporated in vacuo to give a sticky gum. This was rinsed with acetonitrile (80 ml) when a white solid precipitated out. The solid was filtered and dried over phosphorous pentoxide at 60° C. in vacuo for 20 hours to give 32.8 g of the title B compound.

後処理

  1. customThe solvent was evaporated in vacuo
  2. customto give a sticky gum
  3. washThis was rinsed with acetonitrile (80 ml) when a white solid
  4. customprecipitated out
  5. filtrationThe solid was filtered
  6. dry with materialdried over phosphorous pentoxide at 60° C. in vacuo for 20 hours
  7. customto give 32.8 g of the title B compound

出典と根拠

ORDレコード
ord-6a76c51b19744678acb75cc8d37e39e0
出典データセット
uspto-grants-1987_06
特許番号
US04672075

関連ノート

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