Potassium Carbonate → (3AR,8bS)-2-ethoxy-4,8b-dihydro-3aH-indeno[2,1-d]oxazole

HRID 965205ノート

反応式

HRID 965205 の反応式
Cl[C@@H:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH2:4][C@H:3]1[NH:11][C:12]([O:14][CH2:15][CH3:16])=[O:13].C([O-])([O-])=O.[K+].[K+]>C(O)C.O>[CH2:15]([O:14][C:12]1[O:13][C@H:2]2[C:10]3[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=3)[CH2:4][C@H:3]2[N:11]=1)[CH3:16]

参加物

5

反応物 2

HCID 11430Potassium CarbonateHCID 7070371trans-1-Chloro-2-ethoxycarbonylaminoindane

生成物 1

HCID 18661302(3AR,8bS)-2-ethoxy-4,8b-dihydro-3aH-indeno[2,1-d]oxazole

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

A solution of (±) trans-1-chloro-2-ethoxycarbonylaminoindane (B. J. Walker and P. J. Wrobel, J. Chem. Soc. Chem. Commun., 1980, 462)(4.0 g, 0.017 mol) in ethanol (125 ml) was treated with K2CO3 (2.4 g, 0.018 mol) and diluted with water (50 ml). After stirring at room temperature for 20 h, the reaction was concentrated under high vacuum to approximately one quarter the original volume, then diluted with water (25 ml) and extracted into diethyl ether (3×50 ml). The combined extracts were washed with brine, dried over Na2SO4 and concentrated in vacuo to give the title compound as a low melting solid (3.3 g), m.p 53°-54° C. (from diethyl ether/n-pentane).

後処理

  1. concentrationthe reaction was concentrated under high vacuum to approximately one quarter the original volume
  2. additiondiluted with water (25 ml)
  3. extractionextracted into diethyl ether (3×50 ml)
  4. washThe combined extracts were washed with brine
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-99d327fa069d422fadc2dd1db8ddd58a
出典データセット
uspto-grants-1998_06
特許番号
US05773463

反応ノート

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