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Acetic Acid → HCID 15017641、化合物

HRID 2247933
ノート
印刷プレビュー

反応式

HRID 2247933 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([NH:7][C:8]2[S:9][CH:10]=[C:11]([CH2:13][CH2:14][NH2:15])[N:12]=2)[CH:2]=1.[C:16](O)(=O)C.C=O>CO>[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([NH:7][C:8]2[S:9][C:10]3[CH2:16][NH:15][CH2:14][CH2:13][C:11]=3[N:12]=2)[CH:2]=1
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 176Acetic AcidHCID 712Formaldehyde2 回HCID 15017652N-[4-(2-Aminoethyl)-2-thiazolyl]-3-pyridinamine

生成物 1

HCID 15017641HCID 15017641、化合物収率 57.3%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

2-(3-Pyridyl)amino-4-(2-aminoethyl)thiazole (0.50 g, from preceding preparation) and acetic acid (0.19 ml, 3.3 mmol) were dissolved in methanol (23 ml) and treated with formaldehyde (0.19 ml of a 37% aqueous solution, 2.3 mmol). The reaction was allowed to stir at room temperatue for 18 hours, at which point additional formaldehyde (0.02 ml of a 37% aqueous solution, 0.25 mmol) was added. After an additional 2 hours, the reaction mixture was filtered; the filtrate was concentrated in vacuo, dissolved in aqueous base, and extracted with methylene chloride. The organic extracts were dried over sodium sulfate and concentrated to provide the title product (310 mg, 1.3 mmol, 57% yield).

後処理

  1. additionwas added
  2. filtrationthe reaction mixture was filtered
  3. concentrationthe filtrate was concentrated in vacuo
  4. dissolutiondissolved in aqueous base
  5. extractionextracted with methylene chloride
  6. dry with materialThe organic extracts were dried over sodium sulfate
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-4646b92d09f144c6acbc2447f155aaa0
出典データセット
uspto-grants-1991_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05037834

反応ノート

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