Pyridine → 3-Hydroxy-4-(2-pyrrolidin-1-yl-ethoxy)-benzaldehyde O-methyl-oxime

HRID 2236436노트

반응식

HRID 2236436 반응식
[OH:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1[O:10][CH2:11][CH2:12][N:13]1[CH2:17][CH2:16][CH2:15][CH2:14]1)[CH:5]=O.N1C=CC=CC=1.Cl.[O:25]([NH2:27])[CH3:26]>O>[CH3:26][O:25][N:27]=[CH:5][C:4]1[CH:7]=[CH:8][C:9]([O:10][CH2:11][CH2:12][N:13]2[CH2:17][CH2:16][CH2:15][CH2:14]2)=[C:2]([OH:1])[CH:3]=1

참가 물질

5

반응물 3

HCID 1049PyridineHCID 521874O-Methylhydroxylamine hydrochlorideHCID 867611093-Hydroxy-4-(2-pyrrolidin-1-yl-ethoxy)-benzaldehyde

생성물 1

HCID 722507613-Hydroxy-4-(2-pyrrolidin-1-yl-ethoxy)-benzaldehyde O-methyl-oxime수율 59.1%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

An amount of 3-hydroxy-4-(2-pyrrolidin-1-yl-ethoxy)-benzaldehyde (150 mg, 0.64 mmol) is added pyridine (3.5 ml) at room temperature, followed by addition of methoxylamine hydrogen chloride (58.2 mg, 0.70 mmol). The mixture is stirred at ambient temperature for 24 h, and 4 mL of water is added. After the solvents were evaporated, the residue is dissolved 8 mL of anhydrous ether, washed successively with 2 mL of aqueous sodium bicarbonate, 2 mL of sodium bisulfite, and 2 mL of brine. Dried over magnesium sulfate, evaporated to give a yellow solid (100 mg). MS (ESI) m/z 265.8 (M+1)

후처리

  1. customAfter the solvents were evaporated
  2. dissolutionthe residue is dissolved 8 mL of anhydrous ether
  3. washwashed successively with 2 mL of aqueous sodium bicarbonate, 2 mL of sodium bisulfite, and 2 mL of brine
  4. dry with materialDried over magnesium sulfate
  5. customevaporated

출처 및 근거

ORD 기록
ord-d9dca58f60b84c6a9aed32494d028d44
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07713994B2

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