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

HRID 652462

반응식

HRID 652462 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6a76c51b19744678acb75cc8d37e39e0
출처 데이터셋
uspto-grants-1987_06
특허 번호
US04672075

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