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Triethylamine → N-(2-[1-[2-(tert-Butyldiphenylsiloxy)ethyl]cyclohexyl]ethyl)methanesulfonamide

HRID 2223872
ノート
印刷プレビュー

反応式

HRID 2223872 の反応式
[O:1]([CH2:19][CH2:20][C:21]1([CH2:27][CH2:28][NH2:29])[CH2:26][CH2:25][CH2:24][CH2:23][CH2:22]1)[Si:2]([C:15]([CH3:18])([CH3:17])[CH3:16])([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.C(N(CC)CC)C.[CH3:37][S:38](Cl)(=[O:40])=[O:39].C(=O)(O)[O-].[Na+]>ClCCl>[O:1]([CH2:19][CH2:20][C:21]1([CH2:27][CH2:28][NH:29][S:38]([CH3:37])(=[O:40])=[O:39])[CH2:22][CH2:23][CH2:24][CH2:25][CH2:26]1)[Si:2]([C:15]([CH3:17])([CH3:18])[CH3:16])([C:9]1[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 516892Sodium BicarbonateHCID 597149732-[1-[2-(Tert-butyldiphenylsiloxy)ethyl]cyclohexyl]ethylamine

生成物 1

HCID 59714854N-(2-[1-[2-(tert-Butyldiphenylsiloxy)ethyl]cyclohexyl]ethyl)methanesulfonamide

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒

実験手順

To a solution of 2-[1-[2-(tert-butyldiphenylsiloxy)ethyl]cyclohexyl]ethylamine (409 mg) dissolved in dichloromethane (10 mL) was added triethylamine (0.28 mL). Methanesulfonyl chloride (0.12 mL) was added to the solution under ice cooling, and it was stirred at that temperature for 2 hours. Saturated aqueous sodium bicarbonate solution was added to the solution, and it was extracted with chloroform. The organic layer was dried over anhydrous magnesium sulfate, filtered, and then, the solvent was distilled off under reduced pressure. The resulting residue was purified by column chromatography (silica gel, hexane:ethyl acetate=6:1) to give the title compound (327 mg).

後処理

  1. extractionwas extracted with chloroform
  2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  3. filtrationfiltered
  4. distillationthe solvent was distilled off under reduced pressure
  5. customThe resulting residue was purified by column chromatography (silica gel, hexane:ethyl acetate=6:1)

出典と根拠

ORDレコード
ord-5540631c71a74132934b5e529974d45e
出典データセット
uspto-grants-2008_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07375115B2

反応ノート

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