Sodium Thiosulfate → HCID 68609793, 화합물

HRID 1620087노트

반응식

HRID 1620087 반응식
[Br:1]N1C(=O)CCC1=O.[O:9]1[CH2:14][CH2:13][N:12]([C:15]2[N:22]=[CH:21][CH:20]=[CH:19][C:16]=2[C:17]#[N:18])[CH2:11][CH2:10]1.S([O-])([O-])(=O)=S.[Na+].[Na+]>CN(C=O)C>[Br:1][C:20]1[CH:21]=[N:22][C:15]([N:12]2[CH2:13][CH2:14][O:9][CH2:10][CH2:11]2)=[C:16]([CH:19]=1)[C:17]#[N:18]

참가 물질

5

반응물 3

HCID 24477Sodium ThiosulfateHCID 67184N-bromobutanimideHCID 27638522-(Morpholin-4-yl)pyridine-3-carbonitrile

생성물 1

HCID 68609793HCID 68609793, 화합물수율 84.7%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
80 °C

실험 절차

N-bromosuccinimide (141 mg) was added to a DMF (3 ml) solution containing 2-morpholinonicotinonitrile (100 mg), followed by stirring at 80° C. for 5 hours. The reaction solution was adjusted to room temperature. Then, aqueous saturated sodium thiosulfate solution was added, followed by extraction with ethyl acetate. The organic layer was washed with saturated saline and dried over anhydrous sodium sulfate, and then the solvent was distilled away under reduced pressure. The obtained residue was purified by silica gel chromatography (n-hexane:ethyl acetate=10:1 to 7:3), and a light yellow solid of 5-bromo-2-morpholinonicotinonitrile (120 mg) was thus obtained.

후처리

  1. customwas adjusted to room temperature
  2. extractionfollowed by extraction with ethyl acetate
  3. washThe organic layer was washed with saturated saline
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationthe solvent was distilled away under reduced pressure
  6. customThe obtained residue was purified by silica gel chromatography (n-hexane:ethyl acetate=10:1 to 7:3)

출처 및 근거

ORD 기록
ord-0e0a93e444ae41f48ffdf940f453c53a
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08772320B2

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