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Dichloromethane → HCID 178501219、化合物

HRID 926034
ノート
印刷プレビュー

反応式

HRID 926034 の反応式
Cl.[CH:2]([NH:5][C@H:6]1[CH2:11][CH2:10][C@H:9]([C:12]([O:14][CH3:15])=[O:13])[CH2:8][CH2:7]1)([CH3:4])[CH3:3].C(N(CC)CC)C.ClCCl.Cl[S:27]([C:30]1[CH:31]=[C:32]([CH:42]=[CH:43][CH:44]=1)[C:33]([O:35][CH2:36][CH2:37][Si:38]([CH3:41])([CH3:40])[CH3:39])=[O:34])(=[O:29])=[O:28]>N1C=CC=CC=1>[CH:2]([N:5]([C@H:6]1[CH2:11][CH2:10][C@H:9]([C:12]([O:14][CH3:15])=[O:13])[CH2:8][CH2:7]1)[S:27]([C:30]1[CH:31]=[C:32]([CH:42]=[CH:43][CH:44]=1)[C:33]([O:35][CH2:36][CH2:37][Si:38]([CH3:39])([CH3:40])[CH3:41])=[O:34])(=[O:28])=[O:29])([CH3:4])[CH3:3]
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 6344DichloromethaneHCID 8471TriethylamineHCID 866763342-(Trimethylsilyl)ethyl 3-(chlorosulfonyl)benzoateHCID 178501217HCID 178501217、化合物

生成物 1

HCID 178501219HCID 178501219、化合物収率 20.7%

試薬・触媒・溶媒 1

HCID 1049Pyridine
溶媒

実験手順

A mixture of 734 mg of methyl trans-4-(isopropylamino)cyclohexane carboxylate hydrochloride, 0.90 mL of triethylamine, and 10 mL of dichloromethane was stirred at room temperature for 30 minutes, and 10 mL of pyridine and 1.00 g of 2-(trimethylsilyl)ethyl 3-(chlorosulfonyl)benzoate were added thereto in this order, followed by stirring at room temperature overnight. The reaction mixture was concentrated under reduced pressure, and to the residue was added an aqueous citric acid solution, followed by extraction with ethyl acetate. The organic layer was washed with saturated brine, then dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane-ethyl acetate) to obtain 311 mg of 2-(trimethylsilyl)ethyl 3-{isopropyl[trans-4-(methoxycarbonyl)cyclohexyl]sulfamoyl}benzoate as a pale yellow solid. ESI+: 484

後処理

  1. stirringby stirring at room temperature overnight
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. additionto the residue was added an aqueous citric acid solution
  4. extractionfollowed by extraction with ethyl acetate
  5. washThe organic layer was washed with saturated brine
  6. dry with materialdried over anhydrous sodium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customThe residue was purified by silica gel column chromatography (hexane-ethyl acetate)

出典と根拠

ORDレコード
ord-eb94420c38534867907ca8e7dd4952e8
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09284295B2

反応ノート

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