2-Cyanoethanethioamide → HCID 178458231、化合物

HRID 2362823ノート

反応式

HRID 2362823 の反応式
[Si:1]([O:8][CH:9]([CH3:20])[CH2:10][O:11][C:12]1[CH:19]=[CH:18][C:15]([CH:16]=O)=[CH:14][CH:13]=1)([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2].[C:21]([CH2:23][C:24]([NH2:26])=[S:25])#[N:22]>C(O)C>[NH2:26][C:24]1[C:23]([C:21]#[N:22])=[C:16]([C:15]2[CH:18]=[CH:19][C:12]([O:11][CH2:10][CH:9]([O:8][Si:1]([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2])[CH3:20])=[CH:13][CH:14]=2)[C:23]([C:21]#[N:22])=[C:24]([SH:25])[N:26]=1

参加物

4

反応物 2

HCID 14162772-CyanoethanethioamideHCID 592019704-(2-{[tert-Butyl(dimethyl)silyl]oxy}propoxy)benzaldehyde

生成物 1

HCID 178458231HCID 178458231、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 1.77 g (5.99 mmol) of the compound from Example 41A and 1.26 g (12.59 mmol) of cyanothioacetamide in 25 ml of ethanol is stirred at +78° C. for 6 h. The mixture is then cooled to RT and stirred at this temperature for a further 20 h. The resulting precipitate is filtered off with suction and washed with cold diethyl ether. Further product is obtained from the concentrated filtrate solution by chromatographic purification on silica gel 60 (mobile phase gradient cyclohexane/ethyl acetate 1:1→1:4).

後処理

  1. filtrationThe resulting precipitate is filtered off with suction
  2. washwashed with cold diethyl ether
  3. customFurther product is obtained from the concentrated filtrate solution by chromatographic purification on silica gel 60 (mobile phase gradient cyclohexane/ethyl acetate 1:1→1:4)

出典と根拠

ORDレコード
ord-e6df32c03e6e4fce828a081cf8247103
出典データセット
uspto-grants-2014_04
特許番号
US08691850B2

反応ノート

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