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Acetic Anhydride → 2-Methyl-6-acetamidobenzyl alcohol

HRID 2073795
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HRID 2073795 반응식
[NH2:1][C:2]1[CH:9]=[CH:8][CH:7]=[C:6]([CH3:10])[C:3]=1[CH2:4][OH:5].[C:11](OC(=O)C)(=[O:13])[CH3:12].C(=O)(O)[O-].[Na+]>C(Cl)Cl>[CH3:10][C:6]1[CH:7]=[CH:8][CH:9]=[C:2]([NH:1][C:11](=[O:13])[CH3:12])[C:3]=1[CH2:4][OH:5]
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참가 물질

5

반응물 3

HCID 7918Acetic AnhydrideHCID 516892Sodium BicarbonateHCID 15339417(2-Amino-6-methylphenyl)methanol

생성물 1

HCID 143684642-Methyl-6-acetamidobenzyl alcohol수율 64.6%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a suspension of 2-amino-6-methylbenzyl alcohol (30 g) in methylene chloride (300 ml) was added dropwise acetic anhydride (22.3 g) at 5° to 10° C. After being stirred for 3 hours, the mixture was neutralized with sodium bicarbonate aqueous solution to give precipitates. To said mixture was added chloroform to dissolve said precipitates and then the organic layer was washed with water and sodium chloride aqueous solution, dried over magnesium sulfate and evaporated in vacuo. The resultant residue was suspended in diethyl ether and the precipitates were collected by filtration to give 2-methyl-6-acetamidobenzyl alcohol (25.30 g).

후처리

  1. customto give
  2. customprecipitates
  3. additionwas added chloroform
  4. dissolutionto dissolve
  5. customsaid precipitates
  6. washthe organic layer was washed with water and sodium chloride aqueous solution
  7. dry with materialdried over magnesium sulfate
  8. customevaporated in vacuo
  9. filtrationthe precipitates were collected by filtration

출처 및 근거

ORD 기록
ord-a80899f975f149b7b0505acf426b856d
출처 데이터셋
uspto-grants-1990_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04920129

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