Triethylamine → HCID 53968692、化合物

HRID 2289684ノート

反応式

HRID 2289684 の反応式
C(Cl)(=O)C(Cl)=O.[CH:7]([C:10]1[CH:15]=[C:14]([CH:16]([CH3:18])[CH3:17])[CH:13]=[C:12]([CH:19]([CH3:21])[CH3:20])[C:11]=1[CH2:22][C:23](O)=[O:24])([CH3:9])[CH3:8].[S:26](=[O:50])(=[O:49])([O:28][C:29]1[C:34]([CH:35]([CH3:37])[CH3:36])=[CH:33][C:32]([O:38][Si:39]([C:42]([CH3:45])([CH3:44])[CH3:43])([CH3:41])[CH3:40])=[CH:31][C:30]=1[CH:46]([CH3:48])[CH3:47])[NH2:27].C(N(CC)CC)C>C1(C)C=CC=CC=1.CN(C)C=O>[C:42]([Si:39]([CH3:41])([CH3:40])[O:38][C:32]1[CH:31]=[C:30]([CH:46]([CH3:48])[CH3:47])[C:29]([O:28][S:26](=[O:50])(=[O:49])[NH:27][C:23](=[O:24])[CH2:22][C:11]2[C:10]([CH:7]([CH3:8])[CH3:9])=[CH:15][C:14]([CH:16]([CH3:18])[CH3:17])=[CH:13][C:12]=2[CH:19]([CH3:21])[CH3:20])=[C:34]([CH:35]([CH3:37])[CH3:36])[CH:33]=1)([CH3:43])([CH3:45])[CH3:44]

参加物

7

反応物 4

HCID 8471TriethylamineHCID 65578Oxalyl chlorideHCID 105156412,4,6-Triisopropylphenylacetic acidHCID 18698847HCID 18698847、化合物

生成物 1

HCID 53968692HCID 53968692、化合物収率 72.2%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide触媒HCID 1140Toluene溶媒

実験手順

Oxalyl chloride (2.45 mL, 28 mmol) was added dropwise to a solution of 2,4,6-triisopropylphenyl acetic acid (5.66 g, 21.6 mmol) in 150 mL toluene with 4 drops of N,N-dimethylformamide as a catalyst. The resulting solution was stirred for 6 hours and then concentrated in vacuo. The residue was redissolved in 150 mL dichloromethane. 4-(Tert-butyl-dimethyl-silanyloxy)-2,6-diisopropylphenyl sulfamate (8.36 g, 21.6 mmol) and triethylamine (7.5 mL, 54 mmol) were added, and the resulting mixture was stirred overnight. Washed with 1M HCl, dried the organic layer over magnesium sulfate, filtered, and concentrated to give 9.86 g of [(2,4,6-triisopropyl-phenyl)-acetyl]-sulfamic acid 4-(tert-butyl-dimethyl-silanyloxy)-2,6-diisopropyl-phenyl ester.

後処理

  1. concentrationconcentrated in vacuo
  2. dissolutionThe residue was redissolved in 150 mL dichloromethane
  3. stirringthe resulting mixture was stirred overnight
  4. washWashed with 1M HCl
  5. dry with materialdried the organic layer over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-042aa90709b84092be96fe4fe76451ba
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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