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HCID 57712919、化合物 → 5-(2,4-Dimethoxyphenyl)pentanoic acid

HRID 1983428
ノート
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反応式

HRID 1983428 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[CH:6]=[CH:5][C:4]=1/[CH:11]=[CH:12]/[CH2:13][CH2:14][C:15]([OH:17])=[O:16]>C(O)(=O)C>[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[CH:6]=[CH:5][C:4]=1[CH2:11][CH2:12][CH2:13][CH2:14][C:15]([OH:17])=[O:16]
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 57712919HCID 57712919、化合物

生成物 1

HCID 74719765-(2,4-Dimethoxyphenyl)pentanoic acid収率 99%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A 1-L hydrogenation flask was charged with 36.2 g of 5-(2,4-dimethoxyphenyl)-4-pentenoic acid (3a) and 400 ml of glacial acetic acid. The flask was flushed with argon and 2 g of (10% Pd/C) were added to the flask, which was then attached to the hydrogenator. The hydrogenation bottle was evacuated, and charged with hydrogen to 40 to 50 psi. The reaction was run overnight until no further hydrogen was being consumed. The solution was filtered through Cellite (diatomaceous earth). The solvent was evaporated, and the residue dried in vacuo. The yield was 99%. 1H NMR (DMSO-d6) δ: 12.01 (br s, 1H), 6.99 (d, J=8.2 Hz, 1H), 6.49 (d, J=2 Hz, 1H), 6.41 (dd, J1=2 Hz, J2=8.2 Hz, 1H), 3.74 (s, 3H), 3.72 (s, 3H), 2.45 (t, 2H), 2.20 (t, 2H), 1.47 (m, 4H).

後処理

  1. customThe flask was flushed with argon and 2 g of (10% Pd/C)
  2. additionwere added to the flask, which
  3. customThe hydrogenation bottle was evacuated
  4. additioncharged with hydrogen to 40 to 50 psi
  5. customwas being consumed
  6. filtrationThe solution was filtered through Cellite (diatomaceous earth)
  7. customThe solvent was evaporated
  8. customthe residue dried in vacuo

出典と根拠

ORDレコード
ord-f40e430b32904c9da24c15ad3301a74d
出典データセット
uspto-grants-2009_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07541454B2

反応ノート

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