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Sodium amide → 4-Amino-3,5-dimethylbenzaldehyde

HRID 414548
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HRID 414548 반응식
[NH2:1][C:2]1[C:14]([CH3:15])=[CH:13][C:5]([CH:6]([OH:12])CS(C)(=O)=O)=[CH:4][C:3]=1[CH3:16].[NH2-].[Na+]>CS(C)=O>[NH2:1][C:2]1[C:3]([CH3:16])=[CH:4][C:5]([CH:6]=[O:12])=[CH:13][C:14]=1[CH3:15]
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참가 물질

4

반응물 2

HCID 24533Sodium amideHCID 538208514-Amino-3,5-dimethyl-alpha-[(methylsulfonyl)-methyl]-benzyl alcohol

생성물 1

HCID 100347774-Amino-3,5-dimethylbenzaldehyde

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

A solution of 14.6 g. of 4-amino-3,5-dimethyl-α-[(methylsulfonyl)-methyl]-benzyl alcohol in 50 ml. of absolute dimethylsulfoxide was treated with 1.17 g. of sodium amide, stirred for 2 hours at room temperature, diluted with 500 ml. of water and extracted with two 500 ml. portions of ethyl acetate. The ethyl acetate extract was washed with two 200 ml. portions of water and evaporated under vacuum. After recrystallization of the residue from cyclohexane, there was obtained 4-amino-3,5-dimethyl-benzaldehyde having a melting point of 75°-76° C.

후처리

  1. additiondiluted with 500 ml
  2. extractionof water and extracted with two 500 ml
  3. extractionThe ethyl acetate extract
  4. washwas washed with two 200 ml
  5. customportions of water and evaporated under vacuum
  6. customAfter recrystallization of the residue from cyclohexane

출처 및 근거

ORD 기록
ord-667c6f1583fb4d46adc8b6f9345b40ba
출처 데이터셋
uspto-grants-1988_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04792557

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