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Water → HCID 86692469、化合物

HRID 1748520
ノート
印刷プレビュー

反応式

HRID 1748520 の反応式
[OH-].[Na+].O.C([O:6][C:7]([C:9]1([C:19]2[CH:24]=[CH:23][C:22]([Br:25])=[CH:21][N:20]=2)[CH2:18][CH2:17][C:12]2([O:16][CH2:15][CH2:14][O:13]2)[CH2:11][CH2:10]1)=[O:8])C>CO.O1CCCC1>[Br:25][C:22]1[CH:23]=[CH:24][C:19]([C:9]2([C:7]([OH:8])=[O:6])[CH2:10][CH2:11][C:12]3([O:16][CH2:15][CH2:14][O:13]3)[CH2:17][CH2:18]2)=[N:20][CH:21]=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 962WaterHCID 14798Sodium HydroxideHCID 86692455HCID 86692455、化合物

生成物 1

HCID 86692469HCID 86692469、化合物収率 93.5%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

4N Aqueous solution of sodium hydroxide (5 ml) and water (5 ml) were added to a solution of 8-(5-bromopyridin-2-yl)-1,4-dioxaspiro[4,5]decane-8-carboxylic acid ethyl ester (1.0 g) described in Reference Example 81(2) in methanol (10 ml) and tetrahydrofuran (10 ml), and stirred at 80° C. for eight hours. After completion of the reaction, the organic solvent was evaporated and the aqueous layer was washed with diethyl ether. Concentrated hydrochloric acid was added to the aqueous layer under ice cooling, pH was adjusted to 4-5, and extracted with chloroform. The organic layer was dried over anhydrous sodium sulfate and concentrated to give 8-(5-bromopyridin-2-yl)-1,4-dioxaspiro[4,5]decane-8-carboxylic acid (864 mg) as a colorless solid.

後処理

  1. customAfter completion of the reaction
  2. customthe organic solvent was evaporated
  3. washthe aqueous layer was washed with diethyl ether
  4. additionConcentrated hydrochloric acid was added to the aqueous layer under ice cooling
  5. extractionextracted with chloroform
  6. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-5beaceb1fe304717b0f6fe8f314aa667
出典データセット
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09150555B2

反応ノート

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