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Hydrochloric Acid → HCID 178516220、化合物

HRID 491827
ノート
印刷プレビュー

反応式

HRID 491827 の反応式
[O:1]=[C:2]1[CH2:6][CH2:5][CH2:4][N:3]1[C@H:7]1[CH2:12][CH2:11][C@H:10]([C:13]([O:15]C)=[O:14])[CH2:9][CH2:8]1.[OH-].[Na+].Cl.[Cl-].[Na+]>CO>[O:1]=[C:2]1[CH2:6][CH2:5][CH2:4][N:3]1[C@H:7]1[CH2:12][CH2:11][C@H:10]([C:13]([OH:15])=[O:14])[CH2:9][CH2:8]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 4

HCID 313Hydrochloric AcidHCID 5234Sodium ChlorideHCID 14798Sodium HydroxideHCID 178501171HCID 178501171、化合物

生成物 1

HCID 178516220HCID 178516220、化合物収率 97.9%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Methyl trans-4-(2-oxo-pyrrolidin-1-yl)cyclohexanecarboxylate (39.15 g) obtained in Reference Example 113(3) dissolved in methanol (400 ml), and thereto is added 2 N aqueous sodium hydroxide solution (60 ml) and the mixture is stirred at room temperature for 3 hours. The reaction solution is adjusted to pH 1-2 by pouring 10% hydrochloric acid under ice-cooling, saturated with sodium chloride, and then extracted with chloroform. The organic layer is dried over sodium sulfate, and then evaporated to remove the solvent under reduced pressure. The resulting residue is suspended in a small amount of ethyl acetate, and diisopropyl ether is poured thereto, and the resulting crystals are collected by filtration. The crystals are washed with diisopropyl ether several times and dried to give the title compound (35.94 g).

後処理

  1. extractionextracted with chloroform
  2. dry with materialThe organic layer is dried over sodium sulfate
  3. customevaporated
  4. customto remove the solvent under reduced pressure
  5. additionis poured
  6. filtrationthe resulting crystals are collected by filtration
  7. washThe crystals are washed with diisopropyl ether several times
  8. customdried

出典と根拠

ORDレコード
ord-1bd5f03802ac41e1856205f8bb565b72
出典データセット
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07531537B2

反応ノート

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