2-Thiophenecarboxaldehyde → 3-[(Thiophen-2-ylmethyl)-amino]-phthalic acid dimethyl ester

HRID 10037

反応式

HRID 10037 の反応式
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH:6]=O.[CH3:8][O:9][C:10](=[O:27])[C:11]1[C:12](=[C:17]([NH:21]CCCCC)[CH:18]=[CH:19][CH:20]=1)[C:13]([O:15][CH3:16])=[O:14]>>[CH3:8][O:9][C:10](=[O:27])[C:11]1[C:12](=[C:17]([NH:21][CH2:6][C:2]2[S:1][CH:5]=[CH:4][CH:3]=2)[CH:18]=[CH:19][CH:20]=1)[C:13]([O:15][CH3:16])=[O:14]

参加物

3

反応物 2

HCID 73642-ThiophenecarboxaldehydeHCID 210401313-Pentylamino-phthalic acid dimethyl ester

生成物 1

HCID 210401383-[(Thiophen-2-ylmethyl)-amino]-phthalic acid dimethyl ester収率 58%

実験手順

2-Thiophenecarboxaldehyde (1.12 g, 10 mmol) was treated in the same manner as described above for the synthesis of 3-pentylamino-phthalic acid dimethyl ester. The residue (oil) was purified by preparative HPLC (Symmetry C18, isocratic, 45% acetonitrile/water) to give 0.88 g (58%) of yellow oil: 1H NMR (CDCl3) δ 7.38–7.15 (m, 3H), 7.00–6.93 (m, 2H), 6.87–6.82 (m, 2H), 4.58 (d, J=5.3 Hz, 2H), 3.86 (s, 3H), 3.83 (s, 3H).

後処理

  1. customThe residue (oil) was purified by preparative HPLC (Symmetry C18, isocratic, 45% acetonitrile/water)

出典と根拠

ORDレコード
ord-6e253cf5fc8347139a0320e75ea0a5b6
出典データセット
uspto-grants-2006_08
特許番号
US07091353B2

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