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Sulfuric Acid → 2-Benzylindan-2-ylamine

HRID 19729
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HRID 19729 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 1118Sulfuric Acid2회HCID 86611441HCID 86611441, 화합물

생성물 1

HCID 438094522-Benzylindan-2-ylamine

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-28b64453bc6e4d1bb7dc0ff62a5c9670
출처 데이터셋
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07745462B2

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