Bromomethylcyclopropane → 0-Cyclopropylmethyl (2,6-dichlorophenyl)acetamidoxime

HRID 2212057노트

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HRID 2212057 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[CH2:9][C:10](=[N:12][OH:13])[NH2:11].[CH:14]1([CH2:17]Br)[CH2:16][CH2:15]1.CC(C)([O-])C.[K+].P([O-])(O)(O)=O.[Na+]>CN(C)C=O>[CH:14]1([CH2:17][C:4]2([Cl:8])[CH:5]=[CH:6][CH:7]=[C:2]([Cl:1])[CH:3]2[CH2:9][C:10](=[N:12][OH:13])[NH2:11])[CH2:16][CH2:15]1

참가 물질

6

반응물 4

HCID 81503BromomethylcyclopropaneHCID 27581642-(2,6-Dichloro-phenyl)-N-hydroxy-acetamidineHCID 23665647Potassium tert-butoxideHCID 23672064Monosodium phosphate

생성물 1

HCID 1317259160-Cyclopropylmethyl (2,6-dichlorophenyl)acetamidoxime

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

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온도
-20 °C

실험 절차

10.0 g (46 mmol) of (2,6-dichlorophenyl)acetamidoxime in 40 ml of dimethylformamide were admixed with 6.5 g (48 mmol) of cyclopropylmethyl bromide. The mixture was cooled to −20° C. and admixed dropwise with 5.4 g (48 mmol) of potassium tert-butoxide in 20 ml of dimethylformamide. The mixture was stirred at −20° C. for 1 h and then at room temperature overnight, poured into aqueous sodium dihydrogen phosphate buffer (pH 6) and extracted 5 times with diethyl ether. The combined extracts were washed twice with water and once with saturated sodium chloride solution, dried over sodium sulfate and concentrated under reduced pressure. Yield: 12.3 g of a yellow oil which was reacted further without any further purification.

후처리

  1. extractionextracted 5 times with diethyl ether
  2. washThe combined extracts were washed twice with water and once with saturated sodium chloride solution
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customYield: 12.3 g of a yellow oil which was reacted further without any further purification

출처 및 근거

ORD 기록
ord-f1af577398d34c7e9d80b35139659b9f
출처 데이터셋
uspto-grants-2006_09
특허 번호
US07101900B2

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