Tetrabutylammonium Fluoride Trihydrate → HCID 18604777、化合物

HRID 65434

反応式

HRID 65434 の反応式
[CH2:1]([N:4]([CH2:10][S:11]([C:14]([CH3:17])([CH3:16])[CH3:15])(=[O:13])=[O:12])[C:5](=[O:9])[C@@H:6]1[O:8][CH2:7]1)[CH:2]=[CH2:3].[F-].[NH4+].C1COCC1.O.O.O.[F-].C([N+](CCCC)(CCCC)CCCC)CCC>O1CCCC1>[CH2:1]([N:4]1[C@H:10]([S:11]([C:14]([CH3:17])([CH3:16])[CH3:15])(=[O:13])=[O:12])[C@@H:6]([CH2:7][OH:8])[C:5]1=[O:9])[CH:2]=[CH2:3]

参加物

5

反応物 3

HCID 11726816Tetrabutylammonium Fluoride TrihydrateHCID 56993841N-allyl-N-tert.-butylsulphonylmethyl-(R)-glycidic acid amideHCID 69831023ammonium fluoride THF

生成物 1

HCID 18604777HCID 18604777、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of 197 mg (0.757 mmol) of N-allyl-N-tert.-butylsulphonylmethyl-(R)-glycidic acid amide in 1 ml of tetrahydrofuran is introduced at 0°, with the exclusion of moisture, into 8 ml of a tetra-n-butyl; ammonium fluoride/THF solution which has been prepared from 5.0 g of tetra-n-butylammonium fluoride trihydrate by dehydrating at 60° C./0.1 torr and making up to 20 ml with tetrahydrofuran. The reaction mixture is stirred for 2 hours at room temperature and then partitioned between methylene chloride and phosphate buffer solution (pH 8.0). The crude product obtained by drying over sodium sulphate and concentration by evaporation of the organic phase is chromatographed over preparative silica gel plates using hexane/ethyl acetate (1:3). the title compound is obtained in the form of colourless crystals.

後処理

  1. customby dehydrating at 60° C.
  2. custompartitioned between methylene chloride and phosphate buffer solution (pH 8.0)
  3. customThe crude product obtained
  4. dry with materialby drying over sodium sulphate and concentration by evaporation of the organic phase
  5. customis chromatographed over preparative silica gel plates

出典と根拠

ORDレコード
ord-4aba25dbbd1344a8bc8c659123e7942c
出典データセット
uspto-grants-1986_09
特許番号
US04614614

関連ノート

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