2-Cyanoethanethioamide → HCID 178458231, 화합물

HRID 2362823노트

반응식

HRID 2362823 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 178458231HCID 178458231, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-e6df32c03e6e4fce828a081cf8247103
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08691850B2

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