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

HRID 2289685노트

반응식

HRID 2289685 반응식
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

참가 물질

3

반응물 1

HCID 53968692HCID 53968692, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-73bad4f621a34a42aa125a6923d52264
출처 데이터셋
uspto-grants-2000_07
특허 번호
US06093744

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