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Triphenylphosphine → HCID 131720782、化合物

HRID 618835
ノート
印刷プレビュー

反応式

HRID 618835 の反応式
C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.CC(OC(/N=N/C(OC(C)C)=O)=O)C.[Si:34]([O:51][CH2:52][CH:53]([OH:58])[C:54]([O:56][CH3:57])=[O:55])([C:47]([CH3:50])([CH3:49])[CH3:48])([C:41]1[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=1)[C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=1.[C:59](O)(=[S:61])[CH3:60]>C1COCC1>[Si:34]([O:51][CH2:52][CH:53]([O:58][C:59](=[S:61])[CH3:60])[C:54]([O:56][CH3:57])=[O:55])([C:47]([CH3:50])([CH3:49])[CH3:48])([C:41]1[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=1)[C:35]1[CH:36]=[CH:37][CH:38]=[CH:39][CH:40]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 11776TriphenylphosphineHCID 5363146Diisopropyl azodicarboxylateHCID 21255857HCID 21255857、化合物HCID 178418634HCID 178418634、化合物

生成物 1

HCID 131720782HCID 131720782、化合物収率 62%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran
溶媒
2 回

反応条件

温度
0 °C

実験手順

To a solution of triphenylphosphine (101 g, 385 mmol, 2 eq) in THF (1.5 L) was added diisopropylazodicarboxylate (76 mL, 386 mmol, 2 eq) at 0° C. The mixture was stirred at 0° C. for 1 hr and was followed by the addition of a solution of methyl 3-t-butyldiphenylsilyloxy-2-hydroxypropionate (example 39) (68.89 g, 192 mmol) and thioacetic acid (27.6 mL, 386 mmol, 2 eq.) in THF, to the same temperature. The mixture was stirred at 0° C. for 1 hr and at room temperature for 18 hr. The solution was concentrated to dryness and the solid was washed with hexane (5×300 mL). The organic solution was filtered and evaporated under reduced pressure. The crude material was purified by flash chromatography with a mixture of hexane and ethyl acetate (95:5) to give the pure compound (49.3 g) in 62% yield.

後処理

  1. stirringThe mixture was stirred at 0° C. for 1 hr and at room temperature for 18 hr
  2. concentrationThe solution was concentrated to dryness
  3. washthe solid was washed with hexane (5×300 mL)
  4. filtrationThe organic solution was filtered
  5. customevaporated under reduced pressure
  6. customThe crude material was purified by flash chromatography with a mixture of hexane and ethyl acetate (95:5)

出典と根拠

ORDレコード
ord-bcb6b0a14d514eb8b56da8d1652dfa10
出典データセット
uspto-grants-1999_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05955610

反応ノート

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