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Hydrochloric Acid → HCID 68408133、化合物

HRID 505335
ノート
印刷プレビュー

反応式

HRID 505335 の反応式
[NH2:1][C:2]1[C:13]([Cl:14])=[CH:12][CH:11]=[C:10]([Cl:15])[C:3]=1[C:4](N(OC)C)=[O:5].[CH2:16](OCC)C.Cl>C1COCC1.O>[NH2:1][C:2]1[C:13]([Cl:14])=[CH:12][CH:11]=[C:10]([Cl:15])[C:3]=1[C:4](=[O:5])[CH3:16]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 86608958HCID 86608958、化合物

生成物 1

HCID 68408133HCID 68408133、化合物収率 28%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

2-Amino-3,6-dichloro-N-methoxy-N-methyl-benzamide (2491 mg, 10 mmol) were dissolved in THF (100 ml). At −78° C. under nitrogen 1.6 M methyllithium solution in diethylether (25.0 ml, 40 mmol) were added dropwise and the reaction was allowed to reach room temperature and was stirred over night. The reaction was cooled in an icebath and 2N aqueous hydrogen chloride solution (30 ml) were added and the reaction was stirred for 30 min (r.t.). The reaction was diluted with water and extracted twice with diethyl ether. The combined organic layers were washed with saturated aqueous sodium chloride solution, dried over sodium sulfate, filtered and the solvent was evaporated. The residue was purified by column chromatography (CH2Cl2) to yield the product as an orange oil (565 mg, 28%).

後処理

  1. customto reach room temperature
  2. additionwere added
  3. stirringthe reaction was stirred for 30 min (r.t.)
  4. extractionextracted twice with diethyl ether
  5. washThe combined organic layers were washed with saturated aqueous sodium chloride solution
  6. dry with materialdried over sodium sulfate
  7. filtrationfiltered
  8. customthe solvent was evaporated
  9. customThe residue was purified by column chromatography (CH2Cl2)

出典と根拠

ORDレコード
ord-ef072b3d6e5d4885b5a1e158d746ad74
出典データセット
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07781441B2

反応ノート

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