Tetrabutylammonium Fluoride Trihydrate → HCID 18604777, 화합물

HRID 65434

반응식

HRID 65434 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 18604777HCID 18604777, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-4aba25dbbd1344a8bc8c659123e7942c
출처 데이터셋
uspto-grants-1986_09
특허 번호
US04614614

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