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Sodium hydride → HCID 13013062, 화합물

HRID 1194807
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HRID 1194807 반응식
[Cl-].[CH3:2][S+](C)(C)=O.[H-].[Na+].[H][H].[OH:11][C:12]1[CH:19]=[C:18]([CH3:20])[CH:17]=[CH:16][C:13]=1[CH:14]=[O:15]>O1CCCC1.O>[OH:15][CH:14]1[C:13]2[CH:16]=[CH:17][C:18]([CH3:20])=[CH:19][C:12]=2[O:11][CH2:2]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 24758Sodium hydrideHCID 612002-Hydroxy-4-methylbenzaldehydeHCID 197819Trimethyloxosulphonium chlorideHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 13013062HCID 13013062, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매2회

실험 절차

To a solution of trimethylsulfoxonium chloride (12.9 g) in tetrahydrofuran (200 ml) was added sodium hydride (2.4 g of 100%). This solution was heated at reflux until hydrogen evolution had ceased. 13.6 g of 2-hydroxy-4-methylbenzaldehyde dissolved in tetrahydrofuran (100 ml) was then added. The reaction mixture was refluxed until the reaction was complete (3 hours). It was then poured into water (600 ml), extracted with ether, the ether dried over sodium sulphate and evaporated to give 3-hydroxy-6-methyl-2,3-dihydrobenzofuran.

후처리

  1. temperatureThis solution was heated
  2. additionwas then added
  3. temperatureThe reaction mixture was refluxed until the reaction
  4. custom(3 hours)
  5. extractionextracted with ether
  6. dry with materialthe ether dried over sodium sulphate
  7. customevaporated

출처 및 근거

ORD 기록
ord-16e05b46acfe44c8b47b3c671b1a0282
출처 데이터셋
uspto-grants-1989_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04816473

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