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Sodium Sulfate → HCID 14533169, 화합물

HRID 893536
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HRID 893536 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

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

생성물 1

HCID 14533169HCID 14533169, 화합물수율 66%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

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)

후처리

  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

출처 및 근거

ORD 기록
ord-24d0360addc543dc8909dfa71d1063d4
출처 데이터셋
uspto-grants-1992_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05126071

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