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Triethylamine → 4-Methylpiperazine-1-carboxylic acid [4-(2-fluoro-4-nitrophenoxy)pyridin-2-yl]amide

HRID 492677
ノート
印刷プレビュー

反応式

HRID 492677 の反応式
[F:1][C:2]1[CH:15]=[C:14]([N+:16]([O-:18])=[O:17])[CH:13]=[CH:12][C:3]=1[O:4][C:5]1[CH:10]=[CH:9][N:8]=[C:7]([NH2:11])[CH:6]=1.[CH2:19]([N:21]([CH2:24]C)[CH2:22][CH3:23])[CH3:20].ClC([O:29][C:30]1C=CC=CC=1)=O.C[N:37]1CCNCC1>O1CCCC1.C(OCC)(=O)C.CN(C)C=O>[F:1][C:2]1[CH:15]=[C:14]([N+:16]([O-:18])=[O:17])[CH:13]=[CH:12][C:3]=1[O:4][C:5]1[CH:10]=[CH:9][N:8]=[C:7]([NH:11][C:30]([N:37]2[CH2:23][CH2:22][N:21]([CH3:24])[CH2:19][CH2:20]2)=[O:29])[CH:6]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 8471TriethylamineHCID 15891Phenyl chloroformateHCID 531671-MethylpiperazineHCID 231531982-Amino-4-(2-fluoro-4-nitrophenoxy)pyridine

生成物 1

HCID 576774434-Methylpiperazine-1-carboxylic acid [4-(2-fluoro-4-nitrophenoxy)pyridin-2-yl]amide収率 99.9%

試薬・触媒・溶媒 3

HCID 6228
Dimethylformamide
溶媒
HCID 8028Tetrahydrofuran溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 4-(2-fluoro-4-nitrophenoxy)pyridin-2-ylamine (300 mg, 1.2 mmol) and triethylamine (0.335 ml, 2.4 mmol) in tetrahydrofuran (30 ml) was added phenyl chloroformate (0.226 ml, 1.8 mmol) dropwise while stirring in an ice bath, followed by stirring for 1 hr. The reaction mixture was concentrated under a reduced pressure to give a residue, to which was then added N,N-dimethylformamide (6.0 ml) and 1-methylpiperazine (537 μl, 4.84 mmol), followed by stirring at room temperature for 3 hrs. To the reaction mixture was added ethyl acetate (150 ml), washed with a saturated aqueous solution of sodium hydrogencarbonate, and dried over anhydrous sodium sulfate. The solvent was evaporated to give a residue, which was then purified by silica gel column chromatography (Fuji Silysia NH, eluent; hexane:ethyl acetate=1:2, then ethyl acetate) to provide the titled compound (450 mg, 75.3%) as a pale yellow oil.

後処理

  1. stirringby stirring for 1 hr
  2. concentrationThe reaction mixture was concentrated under a reduced pressure
  3. customto give a residue
  4. stirringby stirring at room temperature for 3 hrs
  5. washwashed with a saturated aqueous solution of sodium hydrogencarbonate
  6. dry with materialdried over anhydrous sodium sulfate
  7. customThe solvent was evaporated
  8. customto give a residue, which
  9. customwas then purified by silica gel column chromatography (Fuji Silysia NH, eluent

出典と根拠

ORDレコード
ord-c9c5aa7b9cdd4d98a6e569edab62b464
出典データセット
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07531532B2

反応ノート

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