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Sodium Sulfate → HCID 14533169、化合物

HRID 893536
ノート
印刷プレビュー

反応式

HRID 893536 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[F:7][C:8]([F:19])([F:18])[CH:9]([CH2:14][CH2:15][CH2:16][CH3:17])[CH2:10][C:11](O)=[O:12].S([O-])([O-])(=O)=O.[Na+].[Na+]>CCOCC>[F:7][C:8]([F:18])([F:19])[CH:9]([CH2:14][CH2:15][CH2:16][CH3:17])[CH2:10][CH2:11][OH:12]
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 3

HCID 24436Sodium SulfateHCID 144070633-Trifluoromethylheptanoic acidHCID 21226445Aluminium lithium hydride

生成物 1

HCID 14533169HCID 14533169、化合物収率 66%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

In a two-necked round-bottomed flask replaced with nitrogen, 0.09 g of lithium aluminum hydride and dry ether were placed and cooled with ice, and a solution of 0.5 g of (+)-3-trifluoromethyl-1-heptanoic acid in 3 ml of dry ether was added dropwise thereto. The mixture was stirred for 4 hours on an ice bath for reaction, and a saturated sodium sulfate aqueous solution was added thereto, followed by decantation to recover the ether layer. The ether solution was dried on sodium sulfate, followed by distilling-off of the solvent and distillation by means of a Kugelrohr distiller in the range of 96° C./33 mmHg-104° C./34 mmHg to obtain 290 mg (yield: 66%) of (-)-3-trifluoromethyl-1-heptanol. [α]D21 -2.3 (c 1, CHCl3)

後処理

  1. temperaturecooled with ice
  2. customto recover the ether layer
  3. dry with materialThe ether solution was dried on sodium sulfate
  4. distillationfollowed by distilling-off of the solvent and distillation by means of a Kugelrohr distiller in the range of 96° C./33 mmHg-104° C./34 mmHg

出典と根拠

ORDレコード
ord-24d0360addc543dc8909dfa71d1063d4
出典データセット
uspto-grants-1992_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05126071

反応ノート

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