3-Cyanopyridine → HCID 178513339, 화합물

HRID 908577노트

반응식

HRID 908577 반응식
[C:1](#[N:8])[C:2]1[CH:7]=[CH:6][CH:5]=[N:4][CH:3]=1.Cl.[NH2:10][OH:11].C(=O)([O-])[O-].[Na+].[Na+].[Cl-].[Na+]>O>[OH:11][NH:10][C:1](=[NH:8])[C:2]1[CH:7]=[CH:6][CH:5]=[N:4][CH:3]=1

참가 물질

6

반응물 4

HCID 793-CyanopyridineHCID 5234Sodium ChlorideHCID 10340Sodium CarbonateHCID 443297Hydroxyamine hydrochloride

생성물 1

HCID 178513339HCID 178513339, 화합물

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

Nicotinonitrile (1 g; 10 mmol) and 1.3 g of hydroxylamine hydrochloride (19 mmol) were dissolved in 15 ml of water. Sodium carbonate (2 g; 24 mmol) in 10 ml of water was continuously added, the resulting solution was stirred and heated at app. 70° C. for 6 hours. Then no more starting material was left (checked by TLC), the reaction mixture was cooled to room temperature, added sodium chloride until saturation and extracted 4 times with 50 ml of ethyl acetate. The organic layer was dried with sodium sulfate and evaporated to a solid. Yield 1 g (76%) of white solid powder.

후처리

  1. temperatureheated at app
  2. waitwas left (checked by TLC)
  3. extractionextracted 4 times with 50 ml of ethyl acetate
  4. dry with materialThe organic layer was dried with sodium sulfate
  5. customevaporated to a solid

출처 및 근거

ORD 기록
ord-f2f795451c1a4e75b22d80964e2f0551
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08017631B2

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