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Hydrochloric Acid → HCID 21619378、化合物

HRID 605594
ノート
印刷プレビュー

反応式

HRID 605594 の反応式
[Si:1]([O:18][CH:19]1[CH2:24][CH2:23][CH:22]([C:25]([O:27]CC)=[O:26])[CH2:21][CH2:20]1)([C:14]([CH3:17])([CH3:16])[CH3:15])([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-].[Na+].Cl>CO.O1CCCC1>[Si:1]([O:18][CH:19]1[CH2:20][CH2:21][CH:22]([C:25]([OH:27])=[O:26])[CH2:23][CH2:24]1)([C:14]([CH3:17])([CH3:15])[CH3:16])([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
参加物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 58018637HCID 58018637、化合物

生成物 1

HCID 21619378HCID 21619378、化合物

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 64.2 g of ethyl 4-((tert-butyl(diphenyl)silyl)oxy)cyclohexanecarboxylate in 200 ml of methanol and 200 ml of tetrahydrofuran was added 58 ml of 5 M aqueous sodium hydroxide solution, followed by stirring at room temperature overnight. The reaction mixture was neutralized with 5 M aqueous hydrochloride solution, followed by removal of the methanol and tetrahydrofuran in vacuo, and the resulting residue was extracted with ethyl acetate. The obtained ethyl acetate solution was washed with brine, dried over anhydrous magnesium sulfate and filtered. The filtrate was concentrated in vacuo to give the title compound.

後処理

  1. customfollowed by removal of the methanol and tetrahydrofuran in vacuo
  2. extractionthe resulting residue was extracted with ethyl acetate
  3. washThe obtained ethyl acetate solution was washed with brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. concentrationThe filtrate was concentrated in vacuo

出典と根拠

ORDレコード
ord-9fbcc9cddb5e4511a7ca590798112841
出典データセット
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07915263B2

反応ノート

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