Triethylamine → 3-[(3-Nitro[1,5]naphthyridin-4-yl)amino]propan-1-ol

HRID 1992589노트

반응식

HRID 1992589 반응식
Cl[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][N:10]=2)[N:5]=[CH:4][C:3]=1[N+:12]([O-:14])=[O:13].C(N(CC)CC)C.[NH2:22][CH:23](C)[CH2:24][CH2:25][OH:26]>ClCCl.O>[N+:12]([C:3]1[CH:4]=[N:5][C:6]2[C:11]([C:2]=1[NH:22][CH2:23][CH2:24][CH2:25][OH:26])=[N:10][CH:9]=[CH:8][CH:7]=2)([O-:14])=[O:13]

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 122027913-Aminobutan-1-olHCID 131227874-Chloro-3-nitro-1,5-naphthyridine

생성물 1

HCID 685404393-[(3-Nitro[1,5]naphthyridin-4-yl)amino]propan-1-ol수율 98%

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매

실험 절차

To a solution of 4-chloro-3-nitro[1,5]naphthyridine (18.0 g, 85.9 mmol) in dichloromethane (220 mL) at room temperature was added triethylamine (15.6 mL, 112 mmol) and 3-amino-1-butanol (7.20 mL, 94.5 mmol). The solution was stirred for 4 hours and then was concentrated under reduced pressure to yield an orange solid. The solid was slurried in water (250 mL) for 30 minutes, isolated by filtration, washed with water (3×30 mL), and dried at 70° C. in a vacuum oven to afford 20.9 g of 3-[(3-nitro[1,5]naphthyridin-4-yl)amino]propan-1-ol as a yellow solid.

후처리

  1. concentrationwas concentrated under reduced pressure
  2. customto yield an orange solid
  3. customisolated by filtration
  4. washwashed with water (3×30 mL)
  5. customdried at 70° C. in a vacuum oven

출처 및 근거

ORD 기록
ord-a9f6cb9789d0424e8d656d863c1b4f5a
출처 데이터셋
uspto-grants-2010_01
특허 번호
US07648997B2

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