HCID 18368343、化合物 → HCID 9884882、化合物

HRID 379696ノート

反応式

HRID 379696 の反応式
C(OC([NH:8][CH2:9][CH2:10][O:11][C:12]1[CH:30]=[CH:29][C:15]([NH:16][C:17](=[O:28])[C:18]2[C:23]([O:24][CH3:25])=[CH:22][CH:21]=[CH:20][C:19]=2[O:26][CH3:27])=[CH:14][CH:13]=1)=O)(C)(C)C.Cl.O1CCOCC1>>[NH2:8][CH2:9][CH2:10][O:11][C:12]1[CH:30]=[CH:29][C:15]([NH:16][C:17](=[O:28])[C:18]2[C:19]([O:26][CH3:27])=[CH:20][CH:21]=[CH:22][C:23]=2[O:24][CH3:25])=[CH:14][CH:13]=1

参加物

3

反応物 2

HCID 18368343HCID 18368343、化合物HCID 204431481,4-Dioxane hydrochloride

生成物 1

HCID 9884882HCID 9884882、化合物収率 83.3%

実験手順

4′-[2-(tert-Butoxycarbonylamino)ethoxy]-2,6-dimethoxybenzanilide (1.17 g) was added with 4N HCl/dioxane (5 ml) and mixed for 6 hours at room temperature. The reaction mixture was concentrated under vacuum and residue was dissolved into chloroform (50 ml). The solution was washed with 1N sodium hydroxide aqueous solution (10 ml) followed by saturated sodium chloride (20 ml). After concentration under vacuum to small volume, the solution was subjected to purification by silica-gel column chromatography (chloroform methanol=4:1) to obtain 4′-(2-aminoethoxy)-2,6-dimethoxybenzanilide (0.74 g) as white powder.

後処理

  1. additionmixed for 6 hours at room temperature
  2. concentrationThe reaction mixture was concentrated under vacuum and residue
  3. dissolutionwas dissolved into chloroform (50 ml)
  4. washThe solution was washed with 1N sodium hydroxide aqueous solution (10 ml)
  5. concentrationAfter concentration under vacuum to small volume
  6. customthe solution was subjected to purification by silica-gel column chromatography (chloroform methanol=4:1)

出典と根拠

ORDレコード
ord-99ba9c1f3c4f480ea9a3c9bb1a06c07d
出典データセット
uspto-grants-2001_10
特許番号
US06300368B1

反応ノート

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