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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Water → HCID 20086763、化合物

HRID 1608557
ノート
印刷プレビュー

反応式

HRID 1608557 の反応式
[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[C:4]([CH2:9][C:10](=O)[C:11]2[CH:16]=[CH:15][C:14]([CH2:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[CH:13][CH:12]=2)[C:3]=1[N+:23]([O-:25])=[O:24].C([SiH](CC)CC)C.O>FC(F)(F)C(O)=O>[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[C:4]([CH2:9][CH2:10][C:11]2[CH:16]=[CH:15][C:14]([CH2:17][C:18]([CH3:19])([CH3:20])[CH3:21])=[CH:13][CH:12]=2)[C:3]=1[N+:23]([O-:25])=[O:24]
参加物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 12052Triethylsilane2 回HCID 20086785HCID 20086785、化合物

生成物 1

HCID 20086763HCID 20086763、化合物収率 103.3%

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

A solution of the product from step (b) (11.1 g) in trifluoroacetic acid (16 ml) was stirred at room temperature and triethylsilane (12.5 ml) added. The mixture was stirred overnight at room temperature, followed by 3 hours at 50° C. during which further portions of triethylsilane (3 ml each) were added after 1.5 hours and 2.5 hours, then poured into water (250 ml). The latter was extracted with ether (×2) and the combined extracts washed with water (×2), dried over MgSO4, and evaporated under reduced pressure to give an oil which was flash chromatographed through a silica column using ether/hexane (1:4v/v). The eluate was evaporated under reduced pressure to give 11.0 g of the desired product.

後処理

  1. additionwere added after 1.5 hours and 2.5 hours
  2. extractionThe latter was extracted with ether (×2)
  3. washthe combined extracts washed with water (×2)
  4. dry with materialdried over MgSO4
  5. customevaporated under reduced pressure
  6. customto give an oil which
  7. customchromatographed through a silica column
  8. customThe eluate was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-44a64cdb588344849972137732f71330
出典データセット
uspto-grants-1995_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05395853

反応ノート

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