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Carbon Tetrachloride → HCID 22345410、化合物

HRID 743380
ノート
印刷プレビュー

反応式

HRID 743380 の反応式
[C:1]([Cl:5])(Cl)(Cl)Cl.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[CH3:25][O:26][CH2:27][O:28][C:29]1[CH:36]=[CH:35][CH:34]=[CH:33][C:30]=1CO>O1CCCC1>[CH3:25][O:26][CH2:27][O:28][C:29]1[CH:36]=[CH:35][CH:34]=[CH:33][C:30]=1[CH2:1][Cl:5]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 5943Carbon TetrachlorideHCID 11776TriphenylphosphineHCID 109209042-Methoxymethoxybenzyl alcohol

生成物 1

HCID 22345410HCID 22345410、化合物収率 57%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

16.4 ml of carbon tetrachloride, followed by 44.5 g of triphenylphosphine were added, whilst ice-cooling, to a solution of 23.8 g of 2-methoxymethoxybenzyl alcohol in 240 ml of tetrahydrofuran, and the resulting mixture was heated under reflux for 5 hours. At the end of this time, the mixture was cooled, insoluble materials were filtered off and the filtrate was concentrated by evaporation under reduced pressure. The resulting residue was purified by column chromatography through silica gel, using a 9:1 by volume mixture of hexane and ethyl acetate as the eluent, to give 15.5 g (yield 57%) of the title compound as a colorless liquid.

後処理

  1. additionwere added, whilst ice-
  2. temperaturethe resulting mixture was heated
  3. temperatureunder reflux for 5 hours
  4. temperatureAt the end of this time, the mixture was cooled
  5. filtrationinsoluble materials were filtered off
  6. concentrationthe filtrate was concentrated by evaporation under reduced pressure
  7. customThe resulting residue was purified by column chromatography through silica gel
  8. additionby volume mixture of hexane and ethyl acetate as the eluent

出典と根拠

ORDレコード
ord-9d3c7f253c8240e88b25e7d97ab51fb8
出典データセット
uspto-grants-1996_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05556864

反応ノート

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