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Triethylamine → HCID 140572978、化合物

HRID 2370308
ノート
印刷プレビュー

反応式

HRID 2370308 の反応式
C(OC(=O)[C:5](=[N:7][O:8][CH2:9][CH2:10][CH3:11])[CH3:6])C.[OH-].[Na+].C(Cl)(=O)[C:16](Cl)=[O:17].C(N(CC)CC)C.[NH2:28][C:29]1[CH:34]=[CH:33][CH:32]=[C:31]([CH2:35][O:36]/[N:37]=[C:38](\[C:45]2[N:49]([CH3:50])[N:48]=[N:47][N:46]=2)/[C:39]2[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=2)[N:30]=1>CO.C(Cl)Cl>[CH2:9]([O:8][N:7]=[CH:5][CH2:6][C:16]([NH:28][C:29]1[CH:34]=[CH:33][CH:32]=[C:31]([CH2:35][O:36]/[N:37]=[C:38](\[C:45]2[N:49]([CH3:50])[N:48]=[N:47][N:46]=2)/[C:39]2[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=2)[N:30]=1)=[O:17])[CH2:10][CH3:11]
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 5

HCID 8471TriethylamineHCID 14798Sodium HydroxideHCID 65578Oxalyl chlorideHCID 585674246a({[(Z)a[(1aMethyla1Ha1,2,3,4atetrazola5a yl)(phenyl)methylidene]amino]oxy}methyl)pyridina2a amineHCID 76832219HCID 76832219、化合物

生成物 1

HCID 140572978HCID 140572978、化合物収率 50.9%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6344Dichloromethane溶媒

実験手順

0.12 g (0.70 mmol) of 2-n-propoxyimino-propionic acid ethyl ester was dissolved in 2 ml of methanol and 0.035 g (0.91 mmol) of sodium hydroxide was added to the resulting solution, followed by stirring for 1 hour at room temperature. The solvent was distilled off under reduced pressure, and neutralized with 2N hydrochloric acid, and extracted with chloroform. The organic layer was dried by adding magnesium sulfate, and concentrated tinder reduced pressure to obtain a white solid substance. The white solid substance was dissolved in 5 ml of methylene chloride, and stirred for 40 minutes at room temperature after adding 0.11 g (0.84 mmol) of oxalyl chloride, and concentrated tinder reduced pressure. The residue was dissolved in 5 ml of methylene chloride and stirred for 1 hour at room temperature after adding 0.10 g (0.99 mmol) of triethylamine and 0.14 g (0.45 mmol) of (Z)-(1-methyl-1H-tetrazol-5-yl)phenyl methanone-O-[2-aminopyridin-6-yl methyl]-oxime. The solvent was distilled off and the resulting residue was purified by silica gel column chromatography (eluent: hexane:ethyl acetate=4:1 (v/v)) to obtain 0.10 g of the target compound.

後処理

  1. distillationThe solvent was distilled off under reduced pressure
  2. extractionextracted with chloroform
  3. customThe organic layer was dried
  4. additionby adding magnesium sulfate
  5. concentrationconcentrated tinder reduced pressure
  6. customto obtain a white solid substance
  7. stirringstirred for 40 minutes at room temperature
  8. concentrationconcentrated tinder reduced pressure
  9. dissolutionThe residue was dissolved in 5 ml of methylene chloride
  10. stirringstirred for 1 hour at room temperature
  11. distillationThe solvent was distilled off
  12. customthe resulting residue was purified by silica gel column chromatography (eluent: hexane:ethyl acetate=4:1 (v/v))

出典と根拠

ORDレコード
ord-9c100a68cc064d919005989fdd9c9471
出典データセット
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08710084B2

反応ノート

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