ethyl N-cyanopropionimidate → HCID 178457586、化合物

HRID 2371681ノート

反応式

HRID 2371681 の反応式
[C:1]([N:3]=[C:4](OCC)[CH2:5][CH3:6])#[N:2].[C:10]([C:12]1[CH:25]=[CH:24][C:15]2[O:16][C:17]([CH3:23])([CH3:22])[C@@H:18]([OH:21])[C@H:19]([NH2:20])[C:14]=2[CH:13]=1)#[N:11]>C(OCC)(=O)C>[C:10]([C:12]1[CH:25]=[CH:24][C:15]2[O:16][C:17]([CH3:23])([CH3:22])[C@@H:18]([OH:21])[C@H:19]([NH:20][C:4](=[N:3][C:1]#[N:2])[CH2:5][CH3:6])[C:14]=2[CH:13]=1)#[N:11]

参加物

4

反応物 2

HCID 10820532ethyl N-cyanopropionimidateHCID 10943936(3S,4R)-4-amino-3-hydroxy-2,2-dimethyl-chroman-6-carbonitrile

生成物 1

HCID 178457586HCID 178457586、化合物

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

To 1.39 g of ethyl N-cyanopropionimidate, 2.17 g of 6-cyano-3,4-dihydro-2,2-dimethyl-trans-4-amino-2H-benzo[b]pyran-3-ol was added, and the mixture was reacted under stirring at a temperature of from 100° to 120° C. for 2 hours. The reaction mixture was cooled, then dissolved in 100 ml of ethyl acetate, washed twice with a saturated sodium chloride aqueous solution and then dried over anhydrous sodium sulfate Then, ethyl acetate was distilled off under reduced pressure The residual oily substance was purified by silica gel column chromatography to obtain 1.48 g of the above identified compound in the form of crystals.

後処理

  1. customthe mixture was reacted
  2. temperatureThe reaction mixture was cooled
  3. washwashed twice with a saturated sodium chloride aqueous solution
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationethyl acetate was distilled off under reduced pressure The residual oily substance
  6. customwas purified by silica gel column chromatography
  7. customto obtain 1.48 g of the

出典と根拠

ORDレコード
ord-2a12844b5f2b41e3b8d30b759a484cea
出典データセット
uspto-grants-1992_03
特許番号
US05095016

反応ノート

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