1H-Pyrrolo(2,3-b)pyridine → HCID 22028178, 화합물

HRID 1791145노트

반응식

HRID 1791145 반응식
[NH:1]1[C:5]2=[N:6][CH:7]=[CH:8][CH:9]=[C:4]2[CH:3]=[CH:2]1.[H-].[Na+].Cl.[CH3:13][N:14]([CH3:18])[CH2:15][CH2:16]Cl>CN(C=O)C>[CH3:13][N:14]([CH3:18])[CH2:15][CH2:16][N:1]1[C:5]2=[N:6][CH:7]=[CH:8][CH:9]=[C:4]2[CH:3]=[CH:2]1

참가 물질

5

반응물 3

HCID 92221H-Pyrrolo(2,3-b)pyridineHCID 24758Sodium hydrideHCID 11636816N,N-Dimethylaminoethyl chloride hydrochloride

생성물 1

HCID 22028178HCID 22028178, 화합물수율 81%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A stirred solution of 1H-pyrrolo[2,3-b]pyridine (5.00 g, 42.3 mmol) in DMF at ambient temperature is treated with 95% sodium hydride in oil (3.78 g, 150 mmol). After gas evolution subsides, the reaction mixture is treated with 2-(dimethylamino)-ethyl chloride hydrochloride (6.40 g, 44.4 mmol), stirred for 16 h and concentrated in vacuo. The resultant residue is partitioned between EtOAc and water. The organic phase is separated, dried over MgSO4 and concentrated in vacuo to afford the title compound as an oil, 6.50 g (81% yield), identified by HNMR and mass spectral analyses.

후처리

  1. concentrationconcentrated in vacuo
  2. customThe resultant residue is partitioned between EtOAc and water
  3. customThe organic phase is separated
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-e3364eb7fc144564b9cf7fd10114c659
출처 데이터셋
uspto-grants-2006_07
특허 번호
US07074792B2

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