3,4,5-Trimethoxybenzaldehyde → F1386-0126

HRID 1448950ノート

反応式

HRID 1448950 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:8]=[C:9]([O:13][CH3:14])[C:10]=1[O:11][CH3:12])[CH:6]=O.[N:15]1([CH2:20][CH2:21][NH2:22])[CH:19]=[CH:18][CH:17]=[CH:16]1>C(O)(=O)C>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:6]2[NH:22][CH2:21][CH2:20][N:15]3[CH:19]=[CH:18][CH:17]=[C:16]23)[CH:8]=[C:9]([O:13][CH3:14])[C:10]=1[O:11][CH3:12]

参加物

4

反応物 2

HCID 68583,4,5-TrimethoxybenzaldehydeHCID 27638162-(1H-pyrrol-1-yl)-1-ethanamine

生成物 1

HCID 2770921F1386-0126収率 62.5%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A solution of 3,4,5-trimethoxybenzaldehyde (19.6 g) and 2-(1H-pyrrol-1-yl)ethanamine (11 g, described in Example 7) in acetic acid (250 ml) is stirred at room temperature for 48 hr and evaporated under reduced pressure. The residue is partitioned between chloroform and 10% sodium carbonate and the organic phase is separated, washed with water, dried over magnesium sulfate, filtered and evaporated to give 18 g of the title compound, nmr(CDCl3) δ (2.40(s), 3.35(m), 3.84(s), 3.92(m), 5.03(s), 5.65(m), 6.12(t), 6.61(m) and 6.70(s).

後処理

  1. customevaporated under reduced pressure
  2. customThe residue is partitioned between chloroform and 10% sodium carbonate
  3. customthe organic phase is separated
  4. washwashed with water
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. customevaporated

出典と根拠

ORDレコード
ord-334fae9734624822bb34095114d10e37
出典データセット
uspto-grants-1980_02
特許番号
US04188389

反応ノート

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