Carbon Tetrachloride → HCID 14798665、化合物

HRID 232199ノート

反応式

HRID 232199 の反応式
C(OC(N[C:12]1([C:18]([O:20][CH3:21])=[O:19])[CH2:16][CH2:15][C:14](=[O:17])[O:13]1)=O)C1C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(Cl)(Cl)(Cl)[Cl:42]>>[Cl:42][C:12]1([C:18]([O:20][CH3:21])=[O:19])[CH2:16][CH2:15][C:14](=[O:17])[O:13]1

参加物

4

反応物 3

HCID 5943Carbon TetrachlorideHCID 11776TriphenylphosphineHCID 13995237Methyl 2-benzyloxycarbonylamino-5-oxo-2-tetrahydrofurancarboxylate

生成物 1

HCID 14798665HCID 14798665、化合物

実験手順

A mixture of 80 mg of the Compound (10) obtained in Example 10, 131 mg of triphenylphosphine and 5 ml of carbon tetrachloride was heated under reflux for 4 hours in nitrogen streams. The solvent was evaporated off. The residue was subjected to a flash chromatograph using silica gel, followed by elution with hexane-ethyl acetate (1:2) to give 46 mg of the subject Compound (13) as colorless crystals, m.p. 50.5-51.0° C.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 4 hours in nitrogen streams
  3. customThe solvent was evaporated off
  4. washfollowed by elution with hexane-ethyl acetate (1:2)

出典と根拠

ORDレコード
ord-45a1f0a539c742dd9e4df88b38be0b52
出典データセット
uspto-grants-1989_07
特許番号
US04851422

反応ノート

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