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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Lithium hydroxide, monohydrate → HCID 68537795、化合物

HRID 1442967
ノート
印刷プレビュー

反応式

HRID 1442967 の反応式
[F:1][C:2]1[CH:3]=[C:4]([CH:17]=[CH:18][CH:19]=1)[CH:5]=[C:6]1[CH2:10][N:9]([C:11]([OH:13])=[O:12])[CH:8]([C:14]([OH:16])=[O:15])[CH2:7]1.O.[OH-].[Li+]>O1CCCC1.O>[C:4]([O:12][C:11]([N:9]1[CH2:10][C:6](=[CH:5][C:4]2[CH:17]=[CH:18][CH:19]=[C:2]([F:1])[CH:3]=2)[CH2:7][CH:8]1[C:14]([OH:16])=[O:15])=[O:13])([CH3:17])([CH3:5])[CH3:3]
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 2

HCID 168937Lithium hydroxide, monohydrateHCID 69729930HCID 69729930、化合物

生成物 1

HCID 68537795HCID 68537795、化合物収率 153.2%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a stirred solution of 4-(3-Fluoro-benzylidene)-pyrrolidine-1,2-dicarboxylic acid 1-terf butyl ester 2-methyl ester (3.23 g, 9.63 mmol) in tetrahydrofuran (150 ml), was added 1M lithium hydroxide monohydrate (1.21 g, 28.9 mmol) in water (50 ml). The mixture was stirred at room temperature for 3 days. Tetrahydrofuran was removed by evaporation under reduced pressure, the residue diluted with water (30 ml) and acidified to pH 2.0-3.0 using 1M hydrochloric acid. The aqueous was extracted with diethyl ether (3×100 ml) and the combined organics dried over magnesium sulfate. The solvent was removed by evaporation under reduced pressure to give the title compound (2.37 g, 77%) as a white foam.

後処理

  1. customTetrahydrofuran was removed by evaporation under reduced pressure
  2. additionthe residue diluted with water (30 ml)
  3. extractionThe aqueous was extracted with diethyl ether (3×100 ml)
  4. dry with materialthe combined organics dried over magnesium sulfate
  5. customThe solvent was removed by evaporation under reduced pressure

出典と根拠

ORDレコード
ord-947f058396534d4aa4b9154b30213631
出典データセット
uspto-grants-2010_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07659305B2

反応ノート

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