Acetic Anhydride → N-(6-benzyloxy-3-acetoxy-2,2-dimethylchroman-4-yl)-N-methyl-methanesulfonamide

HRID 613439ノート

反応式

HRID 613439 の反応式
[CH2:1]([O:8][C:9]1[CH:10]=[C:11]2[C:16](=[CH:17][CH:18]=1)[O:15][C:14]([CH3:20])([CH3:19])[CH:13]([OH:21])[CH:12]2[N:22]([CH3:27])[S:23]([CH3:26])(=[O:25])=[O:24])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:28](OC(=O)C)(=[O:30])[CH3:29]>N1C=CC=CC=1>[CH2:1]([O:8][C:9]1[CH:10]=[C:11]2[C:16](=[CH:17][CH:18]=1)[O:15][C:14]([CH3:20])([CH3:19])[CH:13]([O:21][C:28](=[O:30])[CH3:29])[CH:12]2[N:22]([CH3:27])[S:23]([CH3:26])(=[O:24])=[O:25])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 7918Acetic AnhydrideHCID 11760985N-(6-benzyloxy-3-hydroxy-2,2-dimethylchroman-4-yl)-N-methyl-methanesulfonamide

生成物 1

HCID 11048325N-(6-benzyloxy-3-acetoxy-2,2-dimethylchroman-4-yl)-N-methyl-methanesulfonamide

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A solution of 4.5 g of N-(6-benzyloxy-3-hydroxy-2,2-dimethylchroman-4-yl)-N-methyl-methanesulfonamide and 37 ml of acetic anhydride in 74 ml of pyridine was left to stand at RT overnight. The batch was concentrated under reduced pressure and the residue was dissolved in EA, washed successively with dilute hydrochloric acid and saturated sodium bicarbonate solution and dried over magnesium sulfate. Removal of the solvent under reduced pressure gave 4.7 g of N-(6-benzyloxy-3-acetoxy-2,2-dimethylchroman-4-yl)-N-methyl-methanesulfonamide, m.p. 124-125° C.

後処理

  1. concentrationThe batch was concentrated under reduced pressure
  2. dissolutionthe residue was dissolved in EA
  3. washwashed successively with dilute hydrochloric acid and saturated sodium bicarbonate solution
  4. dry with materialdried over magnesium sulfate
  5. customRemoval of the solvent under reduced pressure

出典と根拠

ORDレコード
ord-7edc17a160404fb5a066798cd2568d8b
出典データセット
uspto-grants-1999_12
特許番号
US06008245

反応ノート

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