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Triethylamine → ethyl 2-chloro-N-[[[3,5-dichloro-4-(4-nitrophenoxy)phenyl]amino]carbonyl]benzenecarboximidate

HRID 2198429
ノート
印刷プレビュー

反応式

HRID 2198429 の反応式
[Cl:1][C:2]1[CH:12]=[CH:11][CH:10]=[CH:9][C:3]=1[C:4](=[NH:8])[O:5][CH2:6][CH3:7].[Cl:13][C:14]1[CH:15]=[C:16]([N:31]=[C:32]=[O:33])[CH:17]=[C:18]([Cl:30])[C:19]=1[O:20][C:21]1[CH:26]=[CH:25][C:24]([N+:27]([O-:29])=[O:28])=[CH:23][CH:22]=1.C(N(CC)CC)C>CC(C)=O>[Cl:1][C:2]1[CH:12]=[CH:11][CH:10]=[CH:9][C:3]=1[C:4](=[N:8][C:32]([NH:31][C:16]1[CH:17]=[C:18]([Cl:30])[C:19]([O:20][C:21]2[CH:22]=[CH:23][C:24]([N+:27]([O-:29])=[O:28])=[CH:25][CH:26]=2)=[C:14]([Cl:13])[CH:15]=1)=[O:33])[O:5][CH2:6][CH3:7]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 13092607Ethyl 2-chlorobenzimidateHCID 130926093,5-Dichloro-4-(4-nitrophenoxy)phenylisocyanate

生成物 1

HCID 53641175ethyl 2-chloro-N-[[[3,5-dichloro-4-(4-nitrophenoxy)phenyl]amino]carbonyl]benzenecarboximidate

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A mixture of ethyl 2-chlorobenzimidate hydrofluoroborate (1.90 g., 7.00 mmol), 3,5-dichloro-4-(4-nitrophenoxy)phenylisocyanate (2.28 g., 7.00 mmol) and triethylamine (0.72 g., 7.20 mmol) in acetone (20 ml) is stirred at room temperature for four hours under an atmosphere of dry nitrogen. The reaction mixture is concentrated under reduced pressure and the residue partitioned between ethyl acetate and water. The organic phase is washed sequentially with dilute hydrochloric acid, dilute sodium bicarbonate, and brine. After drying over sodium sulfate, the ethyl acetate solution is concentrated under reduced pressure and the residue chromatographed over silica gel eluting with 20% ethyl acetate in hexane. The product fractions are combined and concentrated under reduced pressure to leave the title compound as an amorphous solid.

後処理

  1. concentrationThe reaction mixture is concentrated under reduced pressure
  2. customthe residue partitioned between ethyl acetate and water
  3. washThe organic phase is washed sequentially with dilute hydrochloric acid, dilute sodium bicarbonate, and brine
  4. dry with materialAfter drying over sodium sulfate
  5. concentrationthe ethyl acetate solution is concentrated under reduced pressure
  6. customthe residue chromatographed over silica gel eluting with 20% ethyl acetate in hexane
  7. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-4600534be54849d1900df576fc0a4526
出典データセット
uspto-grants-1982_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04357347

反応ノート

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