Hydrochloric Acid → HCID 178494574、化合物

HRID 1900061ノート

反応式

HRID 1900061 の反応式
[OH:1][C@H:2]1[CH2:7][CH2:6][C@H:5]([C:8]2[CH:13]=[CH:12][C:11]([N:14]3[CH2:18][CH:17]([CH2:19][O:20][CH3:21])[O:16][C:15]3=[O:22])=[CH:10][CH:9]=2)[CH2:4][CH2:3]1.Cl[CH:24]([C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1)[C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1.Cl>C(N(C(C)C)C(C)C)C>[CH:24]([O:1][C@H:2]1[CH2:7][CH2:6][C@H:5]([C:8]2[CH:9]=[CH:10][C:11]([N:14]3[CH2:18][CH:17]([CH2:19][O:20][CH3:21])[O:16][C:15]3=[O:22])=[CH:12][CH:13]=2)[CH2:4][CH2:3]1)([C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1)[C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 7035ChlorodiphenylmethaneHCID 178494572HCID 178494572、化合物

生成物 1

HCID 178494574HCID 178494574、化合物

試薬・触媒・溶媒 1

HCID 81531Diisopropylethylamine溶媒

実験手順

0.5 g of (RS)-3-[4-(trans-4-hydroxy-cyclohexyl)-phenyl]-5-methoxymethyl-oxazolidin-2-one in 5 ml of ethyldiisopropylamine was heated with 0.35 ml of chlorodiphenylmethane to 100° and stirred at this temperature for 7 hours. The reaction mixture was cooled, acidified with 1N hydrochloric acid and extracted with ethyl acetate. The organic phase was washed neutral with water, dried with magnesium sulfate and concentrated. The residue (0.7 g) was chromatographed on a 30-fold amount of silica gel with methylene chloride/ethyl acetate mixtures. 0.3 g of (RS)-3-[4-(trans-4-benzhydryloxy-cyclohexyl)-phenyl]-5-methoxymethyl-oxazolidin-2-one was obtained as colorless crystals. M.p.: 146°-148°.

後処理

  1. temperatureThe reaction mixture was cooled
  2. extractionextracted with ethyl acetate
  3. washThe organic phase was washed neutral with water
  4. dry with materialdried with magnesium sulfate
  5. concentrationconcentrated
  6. customThe residue (0.7 g) was chromatographed on a 30-fold amount of silica gel with methylene chloride/ethyl acetate mixtures

出典と根拠

ORDレコード
ord-796d3578c5a3405682388bd5af1787c8
出典データセット
uspto-grants-1996_11
特許番号
US05574055

反応ノート

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