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Acetic Acid → HCID 15017641, 화합물

HRID 249301
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HRID 249301 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 712Formaldehyde2회HCID 15017652N-[4-(2-Aminoethyl)-2-thiazolyl]-3-pyridinamine

생성물 1

HCID 15017641HCID 15017641, 화합물수율 57.3%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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 temperature 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).

후처리

  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

출처 및 근거

ORD 기록
ord-085488d602404228a106cab0f6201258
출처 데이터셋
uspto-grants-1993_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05214051

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