2-Amino-2-methylpropionitrile → hexahydro-1H-pyrrolizine-7a-carbonitrile
反応式
[NH2:1][C:2](C)(C)C#N.Cl[CH2:8][CH2:9][CH2:10][C:11](=O)[CH2:12][CH2:13][CH2:14]Cl.[NH3:17].CO>>[C:2]([C:11]12[CH2:12][CH2:13][CH2:14][N:17]1[CH2:8][CH2:9][CH2:10]2)#[N:1]参加物
4
実験手順
A mixed solution of 2-amino-2-methylpropanenitrile (41.4 g, 492 mmol) and 1,7-dichloro-4-heptanone (30.0 g, 164 mmol) in 220 ml of 16% NH3 /MeOH solution was stirred for 24 hours at 20° C. The resulting reaction mixture was concentrated in vacuo to remove MeOH therefrom, added 0.1N NaOH to the residue, which was extracted with methylene chloride, and the extract was dried over anhydrous sodium sulfate, concentrated, and distilled in vacuo to afford 18.1 g of the desired compound (Yield: 82%).
後処理
- customThe resulting reaction mixture
- concentrationwas concentrated in vacuo
- customto remove MeOH
- additionadded 0.1N NaOH to the residue, which
- extractionwas extracted with methylene chloride
- dry with materialthe extract was dried over anhydrous sodium sulfate
- concentrationconcentrated
- distillationdistilled in vacuo
出典と根拠
- ORDレコード
- ord-141bd7dd0c4740a2b76f057e5fe7379d
- 出典データセット
- uspto-grants-1990_01
- 特許番号
- US04897495
反応ノート
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