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Water → HCID 59389336、化合物

HRID 2357943
ノート
印刷プレビュー

反応式

HRID 2357943 の反応式
[F-].C([N+](CCCC)(CCCC)CCCC)CCC.O1CCCC1.[Si]([O:31][CH2:32][C:33]1[C:34]2[N:35]([N:42]=[C:43]([C:45]([F:48])([F:47])[F:46])[CH:44]=2)[C:36]([CH2:39][O:40][CH3:41])=[CH:37][CH:38]=1)(C(C)(C)C)(C)C.O>O1CCCC1>[OH:31][CH2:32][C:33]1[C:34]2[N:35]([N:42]=[C:43]([C:45]([F:48])([F:47])[F:46])[CH:44]=2)[C:36]([CH2:39][O:40][CH3:41])=[CH:37][CH:38]=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

5

反応物 3

HCID 962WaterHCID 11078149TBAF tetrahydrofuranHCID 58014019HCID 58014019、化合物

生成物 1

HCID 59389336HCID 59389336、化合物収率 98.6%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

A 1 mol/L tetrabutylammonium fluoride-tetrahydrofuran solution (35.1 mL) was added dropwise to a solution of the compound of Example 325 (8.76 g) in tetrahydrofuran (120 mL) at 0° C. The mixture was stirred at 0° C. for 30 min. Subsequently, water was added and the mixture was extracted with ethyl acetate (300 mL). The organic layer was washed sequentially with water and saturated brine and dried over anhydrous sodium sulfate. The extract was concentrated and purified by silica gel column chromatography (hexane:ethyl acetate=3:1) to afford the title compound as a colorless powder (6.00 g).

後処理

  1. extractionthe mixture was extracted with ethyl acetate (300 mL)
  2. washThe organic layer was washed sequentially with water and saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationThe extract was concentrated
  5. custompurified by silica gel column chromatography (hexane:ethyl acetate=3:1)

出典と根拠

ORDレコード
ord-b31e7e7e7c5642df8701eddff4ac7773
出典データセット
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07763617B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート