2-Amino-2-methylpropionitrile → hexahydro-1H-pyrrolizine-7a-carbonitrile

HRID 330593

反応式

HRID 330593 の反応式
[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

反応物 3

HCID 880222-Amino-2-methylpropionitrileHCID 2467491,7-Dichloro-heptan-4-oneHCID 21705897Ammonia methanol

生成物 1

HCID 11029899hexahydro-1H-pyrrolizine-7a-carbonitrile収率 82%

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

  1. customThe resulting reaction mixture
  2. concentrationwas concentrated in vacuo
  3. customto remove MeOH
  4. additionadded 0.1N NaOH to the residue, which
  5. extractionwas extracted with methylene chloride
  6. dry with materialthe extract was dried over anhydrous sodium sulfate
  7. concentrationconcentrated
  8. 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

関連ノート

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