反応式
[C:1]([O:5][C:6]([C:8]1[C:16]2[CH2:15][CH2:14][O:13][CH:12]([CH2:17][N:18]3C(=O)C4C(=CC=CC=4)C3=O)[C:11]=2[S:10][C:9]=1[NH2:29])=[O:7])([CH3:4])([CH3:3])[CH3:2].O.NN>C(O)C>[C:1]([O:5][C:6]([C:8]1[C:16]2[CH2:15][CH2:14][O:13][CH:12]([CH2:17][NH2:18])[C:11]=2[S:10][C:9]=1[NH2:29])=[O:7])([CH3:4])([CH3:2])[CH3:3]参加物
4
反応物 2
生成物 1
試薬・触媒・溶媒 1
実験手順
To a mixture of 2-amino-7-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4,7-dihydro-5H-thieno[2,3-c]pyran-3-carboxylic acid tert-butyl ester (6.0 g, 0.014 mol) in ethanol (100 ml) was added hydrazine hydrate (1.4 ml, 0.028 mol). The reaction mixture was heated at reflux for 1 h, cooled and the precipitate filtered off. The filtrate was evaporated in vacuo and to the residue was added water (100 ml) and the resulting mixture was extracted with diethyl ether (2×100 ml). The combined organic extracts were washed with brine (100 ml), dried (Na2SO4), filtered and the solvent evaporated in vacuo affording 2.9 g (71%) of 2-amino-7-aminomethyl-4,7-dihydro-5H-thieno[2,3-c]pyran-3-carboxylic acid tert-butyl ester as an oil.
後処理
- temperatureThe reaction mixture was heated
- temperatureat reflux for 1 h
- temperaturecooled
- filtrationthe precipitate filtered off
- customThe filtrate was evaporated in vacuo and to the residue
- additionwas added water (100 ml)
- extractionthe resulting mixture was extracted with diethyl ether (2×100 ml)
- washThe combined organic extracts were washed with brine (100 ml)
- dry with materialdried (Na2SO4)
- filtrationfiltered
- customthe solvent evaporated in vacuo
出典と根拠
- ORDレコード
- ord-f9db52eb2df449d69cfdffb8226365e5
- 出典データセット
- uspto-grants-2005_10
- 特許番号
- US06951878B2
関連ノート
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