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Sulfuric Acid → 2-Benzylindan-2-ylamine

HRID 19729
ノート
印刷プレビュー

反応式

HRID 19729 の反応式
[CH2:1]([C:8]1([NH:18]C(=O)C(F)(F)F)[CH2:16][C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[C:9]1=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.OS(O)(=O)=O>C(O)(=O)C>[CH2:1]([C:8]1([NH2:18])[CH2:16][C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[CH2:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
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 1118Sulfuric Acid2 回HCID 86611441HCID 86611441、化合物

生成物 1

HCID 438094522-Benzylindan-2-ylamine

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A mixture of N-(2-benzyl-1-oxoindan-2-yl)-2,2,2-trifluoroacetamide (0.200 g, 0.60 mmol), 10% Pdl/C (50 mg) and concentrated H2SO4 (30 μl) in acetic acid (13.3 ml) is hydrogenated at 0.35 bar for 1 hour. Further concentrated H2SO4 (10 μl) is added and the hydrogenation is continued for 16 hours. The reaction is filtered, the filtrate is evaporated and the residue partitioned between ethyl acetate and water. The aqueous phase is basified to pH 11 with 1 M aqueous NaOH and extracted with ethyl acetate. The organic extract is washed with brine, dried (MgSO4) and evaporated to afford 2-benzylindan-2-ylamine, MH+ 224.

後処理

  1. waitthe hydrogenation is continued for 16 hours
  2. filtrationThe reaction is filtered
  3. customthe filtrate is evaporated
  4. customthe residue partitioned between ethyl acetate and water
  5. extractionextracted with ethyl acetate
  6. extractionThe organic extract
  7. washis washed with brine
  8. dry with materialdried (MgSO4)
  9. customevaporated

出典と根拠

ORDレコード
ord-28b64453bc6e4d1bb7dc0ff62a5c9670
出典データセット
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07745462B2

反応ノート

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