Pyridine → HCID 10365880, 화합물

HRID 247963

반응식

HRID 247963 반응식
[NH2:1][CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][N:4]=1.N1C=CC=CC=1.[CH2:15]([O:29][C:30]1[CH:35]=[CH:34][C:33]([CH2:36][C:37](Cl)=[O:38])=[CH:32][CH:31]=1)[CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28]>C(Cl)Cl.C(Cl)(Cl)Cl>[N:4]1[CH:5]=[CH:6][CH:7]=[CH:8][C:3]=1[CH2:2][NH:1][C:37](=[O:38])[CH2:36][C:33]1[CH:34]=[CH:35][C:30]([O:29][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28])=[CH:31][CH:32]=1

참가 물질

6

반응물 3

HCID 1049PyridineHCID 195092-PyridinemethanamineHCID 10021844p-Tetradecyloxyphenylacetylchloride

생성물 1

HCID 10365880HCID 10365880, 화합물수율 61.3%

시약·촉매·용매 2

HCID 6212Chloroform용매HCID 6344Dichloromethane용매2회

반응 조건

온도
0 °C

실험 절차

To a 0° C. solution of 4.64 g of 2-(aminomethyl)pyridine, 13.2 ml of pyridine and 50 ml of methylene chloride is added, dropwise, 15 g of product from Example 53 in 150 ml of methylene chloride. The reaction is stirred at 0° C. for 1 hour followed by 18 hours at room temperature. The reaction is diluted with chloroform, washed with sodium bicarbonate, water and saturated sodium chloride, dried and concentrated in vacuo. The residue is purified by column chromatography (silica gel:75-100% ethyl acetate/hexane) to give 11.0 g of the desired product as colorless prisms.

후처리

  1. waitfollowed by 18 hours at room temperature
  2. washwashed with sodium bicarbonate, water and saturated sodium chloride
  3. customdried
  4. concentrationconcentrated in vacuo
  5. customThe residue is purified by column chromatography (silica gel:75-100% ethyl acetate/hexane)

출처 및 근거

ORD 기록
ord-a1bf0a5df96747c39599d0ba2a93f7d4
출처 데이터셋
uspto-grants-1993_05
특허 번호
US05208247

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