HCID 53968692、化合物 → [(2,4,6-Triisopropyl-phenyl)-acetyl]-sulfamic acid 4-hydroxy-2,6-diisopropyl-phenyl ester

HRID 2289685ノート

反応式

HRID 2289685 の反応式
C([Si](C)(C)[O:6][C:7]1[CH:12]=[C:11]([CH:13]([CH3:15])[CH3:14])[C:10]([O:16][S:17](=[O:38])(=[O:37])[NH:18][C:19](=[O:36])[CH2:20][C:21]2[C:26]([CH:27]([CH3:29])[CH3:28])=[CH:25][C:24]([CH:30]([CH3:32])[CH3:31])=[CH:23][C:22]=2[CH:33]([CH3:35])[CH3:34])=[C:9]([CH:39]([CH3:41])[CH3:40])[CH:8]=1)(C)(C)C>C(#N)C>[OH:6][C:7]1[CH:8]=[C:9]([CH:39]([CH3:41])[CH3:40])[C:10]([O:16][S:17](=[O:38])(=[O:37])[NH:18][C:19](=[O:36])[CH2:20][C:21]2[C:22]([CH:33]([CH3:34])[CH3:35])=[CH:23][C:24]([CH:30]([CH3:31])[CH3:32])=[CH:25][C:26]=2[CH:27]([CH3:29])[CH3:28])=[C:11]([CH:13]([CH3:15])[CH3:14])[CH:12]=1

参加物

3

反応物 1

HCID 53968692HCID 53968692、化合物

生成物 1

HCID 10142635[(2,4,6-Triisopropyl-phenyl)-acetyl]-sulfamic acid 4-hydroxy-2,6-diisopropyl-phenyl ester収率 90.8%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A solution of 15 mL concentrated HF in 150 mL acetonitrile was added dropwise to a solution of [(2,4,6-triisopropyl-phenyl)-acetyl]-sulfamic acid 4-(tert-butyl-dimethyl-silanyloxy)-2,6-diisopropyl-phenyl ester (9.71 g, 15.4 mmol) in 400 mL acetonitrile at room temperature under a nitrogen atmosphere. Stirred for 16 hours and then concentrated in vacuo. The residue was partitioned between water and dichloromethane. The organic layer was dried over magnesium sulfate, filtered, and concentrated to give an oily solid. Trituration with hexanes gave 7.24 g of [(2,4,6-triisopropyl-phenyl)-acetyl]-sulfamic acid 4-hydroxy-2,6-diisopropyl-phenyl ester as a white solid; mp 182-183° C.

後処理

  1. concentrationA solution of 15 mL concentrated HF in 150 mL acetonitrile
  2. concentrationconcentrated in vacuo
  3. customThe residue was partitioned between water and dichloromethane
  4. dry with materialThe organic layer was dried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customto give an oily solid

出典と根拠

ORDレコード
ord-73bad4f621a34a42aa125a6923d52264
出典データセット
uspto-grants-2000_07
特許番号
US06093744

反応ノート

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