Sodium hydride → 1,1-Bis(diisopropoxyphosphinoyl)-3-triphenylmethoxypropane

HRID 1737290

반응식

HRID 1737290 반응식
[H-].[Na+].Br[CH2:4][CH2:5][O:6][C:7]([C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.[CH2:26]([P:37](=[O:46])([O:42][CH:43]([CH3:45])[CH3:44])[O:38][CH:39]([CH3:41])[CH3:40])[P:27](=[O:36])([O:32][CH:33]([CH3:35])[CH3:34])[O:28][CH:29]([CH3:31])[CH3:30].[Cl-].[NH4+]>C1(C)C=CC=CC=1.C(OCC)(=O)C>[CH:39]([O:38][P:37]([O:42][CH:43]([CH3:45])[CH3:44])([CH:26]([P:27]([O:32][CH:33]([CH3:35])[CH3:34])([O:28][CH:29]([CH3:30])[CH3:31])=[O:36])[CH2:4][CH2:5][O:6][C:7]([C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)=[O:46])([CH3:41])[CH3:40]

참가 물질

7

반응물 4

HCID 24758Sodium hydride2회HCID 25517Ammonium ChlorideHCID 74266Tetraisopropyl methylenediphosphonateHCID 10959531HCID 10959531, 화합물

생성물 1

HCID 218419981,1-Bis(diisopropoxyphosphinoyl)-3-triphenylmethoxypropane수율 77.4%

시약·촉매·용매 2

HCID 1140Toluene용매2회HCID 8857Ethyl Acetate용매

반응 조건

온도
120 °C

실험 절차

Under a nitrogen atmosphere, 60% sodium hydride (200 mg), 1-bromo-2-triphenylmethoxyethane (1.84 g) and tetraisopropyl methylenebisphosphonate (1.72 g) were suspended in toluene (5 ml), and the resulting suspension was stirred at 120° C. for 7 hours. The reaction mixture was diluted with toluene, and then a saturated aqueous ammonium chloride solution was added thereto to decompose the excess sodium hydride. Then, ethyl acetate was added thereto to effect separation, and the organic layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified by a silica gel column chromatography (chloroform:acetone) to obtain 1,1-bis(diisopropoxyphosphinoyl)-3-triphenylmethoxypropane (2.44 g, yield 77%).

후처리

  1. customseparation
  2. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customThe residue was purified by a silica gel column chromatography (chloroform:acetone)

출처 및 근거

ORD 기록
ord-3d253bd6539e4ec89bb0faf99b9f6fb4
출처 데이터셋
uspto-grants-1999_10
특허 번호
US05962438

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