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Hydrochloric Acid → HCID 178527049、化合物

HRID 1292575
ノート
印刷プレビュー

反応式

HRID 1292575 の反応式
[OH-].[Na+].[C:3]1([P:9]([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[C:10]2[CH:15]=[CH:14][C:13]([CH2:16][PH:17](=[O:23])[O:18]CC(C)C)=[CH:12][CH:11]=2)[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.Cl>O.C1COCC1>[C:3]1([P:9]([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[C:10]2[CH:15]=[CH:14][C:13]([CH2:16][PH:17](=[O:18])[OH:23])=[CH:12][CH:11]=2)[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=1
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

6

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 178454801HCID 178454801、化合物

生成物 1

HCID 178527049HCID 178527049、化合物収率 95.6%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
23 °C

実験手順

8.70 g (2127.5 mmol) of NaOH in 40 ml of water were added dropwise at 23° C. to a solution of 34.52 g (87 mmol) of isobutyl (4-diphenylphosphino-phenyl)methylphosphinate in 50 ml of THF. After heating under reflux for 6 hours, 18.1 ml (218 mmol) of concentrated hydrochloric acid were added dropwise at 23° C., the mixture was stirred for 10 minutes at 23° C. and completely evaporated on a rotary evaporator. The residue is taken up in methylene chloride, the solution was dried over Na2SO4 and completely evaporated. Drying under reduced pressure gave 28.3 g of (4-diphenylphosphinophenyl)methylphosphinic acid (90% of theory) in the form of a pale yellow solid having a melting point of 40° C.

後処理

  1. temperatureAfter heating
  2. temperatureunder reflux for 6 hours
  3. customcompletely evaporated on a rotary evaporator
  4. dry with materialthe solution was dried over Na2SO4
  5. customcompletely evaporated
  6. customDrying under reduced pressure

出典と根拠

ORDレコード
ord-3e8d43dea4e343b591f9566e17e9c33d
出典データセット
uspto-grants-1998_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05756804

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート