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Hydrochloric Acid → HCID 12082058、化合物

HRID 1760354
ノート
印刷プレビュー

反応式

HRID 1760354 の反応式
C([Li])CCC.[O:6]1[CH2:10][CH2:9][CH2:8][C@@H:7]1[C:11]#N.Cl.[O:14]1[CH2:18][CH2:17][CH2:16][CH2:15]1>CCCCCC.O>[O:14]1[CH2:18][CH2:17][CH2:16][C@@H:15]1[C:10](=[O:6])[CH2:9][CH2:8][CH2:7][CH3:11]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 8028TetrahydrofuranHCID 7204860(R)-Tetrahydrofuran-2-carbonitrileHCID 178418339Butyllithium

生成物 1

HCID 12082058HCID 12082058、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8058
Hexane
溶媒

実験手順

A 1 L reactor at a temperature of 0° C. was added with 0.4 L of 1.6 M n-butyllithium in n-hexane, to which 13.5 g of (R)-2-tetrahydrofuran nitrile as previously obtained, in 0.07 L of tetrahydrofuran was slowly added dropwise. As such, the reaction was carried out for 1 hour with stirring, while the temperature within the reactor was controlled below 15° C. Next, the resulting solution was added dropwise to 65 g of concentrated hydrochloric acid in 0.4 L of water, while the temperature of the reaction was controlled below 25° C. Thereafter, the extraction was conducted by use of ethylacetate, followed by removing the solvent therein under reduced pressure, and the remainder was vacuum distilled off to produce 19.6 g of (R)-1-(2-tetrahydrofuranyl)-1-pentanone having an optical purity of 98.5% ee.

後処理

  1. additionwas slowly added dropwise
  2. customwas controlled below 15° C
  3. customwas controlled below 25° C
  4. extractionThereafter, the extraction
  5. customby removing the solvent
  6. distillationdistilled off

出典と根拠

ORDレコード
ord-80b99ff642254f31a5c535c8dde0bc85
出典データセット
uspto-grants-2005_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06841688B2

反応ノート

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