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

HRID 1992589ノート

反応式

HRID 1992589 の反応式
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]

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a9f6cb9789d0424e8d656d863c1b4f5a
出典データセット
uspto-grants-2010_01
特許番号
US07648997B2

反応ノート

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