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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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Ammonium Hydroxide → HCID 57562895、化合物

HRID 1725667
ノート
印刷プレビュー

反応式

HRID 1725667 の反応式
Cl[S:2]([C:5]1[CH:6]=[C:7]([N+:13]([O-:15])=[O:14])[CH:8]=[C:9]([CH3:12])[C:10]=1[F:11])(=[O:4])=[O:3].[OH-].[NH4+:17]>C(OCC)(=O)C>[NH2:17][S:2]([C:5]1[CH:6]=[C:7]([N+:13]([O-:15])=[O:14])[CH:8]=[C:9]([CH3:12])[C:10]=1[F:11])(=[O:4])=[O:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14923Ammonium HydroxideHCID 575628802-Fluoro-3-methyl-5-nitrobenzene-1-sulfonyl chloride

生成物 1

HCID 57562895HCID 57562895、化合物

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

The resulting oily residue of compound 26 was taken up in ethyl acetate (100 mL) and stirred with ammonium hydroxide (100 mL, 30% aqueous solution) overnight at room temperature. After the ethyl acetate layer was separated, the aqueous layer was extracted with ethyl acetate (2×50 mL). The organic layers were combined, dried over anhydrous sodium sulfate and the solvent was removed under vacuum. The dark oily residue was chromatographed (silica gel, hexanes then 10%, 20%, up to 50% ethyl acetate in hexanes to afford 3-aminosulfonyl-4-fluoro-5-methylnitrobenzene (27). LCMS: purity: 89%; MS (m/z): 235 (MH+).

後処理

  1. customAfter the ethyl acetate layer was separated
  2. extractionthe aqueous layer was extracted with ethyl acetate (2×50 mL)
  3. dry with materialdried over anhydrous sodium sulfate
  4. customthe solvent was removed under vacuum
  5. customThe dark oily residue was chromatographed (silica gel, hexanes

出典と根拠

ORDレコード
ord-aaae855d4a2c41349957d8a7597ac04a
出典データセット
uspto-grants-2009_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07491732B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート