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

HRID 1737290
ノート
印刷プレビュー

反応式

HRID 1737290 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 24758Sodium hydride2 回HCID 25517Ammonium ChlorideHCID 74266Tetraisopropyl methylenediphosphonateHCID 109595312-Bromoethyl trityl ether

生成物 1

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

試薬・触媒・溶媒 2

HCID 1140
Toluene
溶媒
2 回
HCID 8857Ethyl Acetate溶媒

反応条件

温度
120 °C

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-3d253bd6539e4ec89bb0faf99b9f6fb4
出典データセット
uspto-grants-1999_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05962438

反応ノート

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