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Acetic Acid → HCID 15017643, 화합물

HRID 249303
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HRID 249303 반응식
[CH3:1][N:2]([CH3:11])[C:3]1[S:4][CH:5]=[C:6]([CH2:8][CH2:9][NH2:10])[N:7]=1.C=O.[C:14](O)(=O)C>O.CO>[CH3:11][N:2]([CH3:1])[C:3]1[S:4][C:5]2[CH2:14][NH:10][CH2:9][CH2:8][C:6]=2[N:7]=1
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참가 물질

6

반응물 3

HCID 176Acetic AcidHCID 712Formaldehyde2회HCID 15017654124458-20-4

생성물 1

HCID 15017643HCID 15017643, 화합물수율 219.2%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

2-Dimethylamino-4-(2-aminoethyl)thiazole (1.7 g, see preceding preparation), formaldehyde (0.78 ml of a 37% solution in water, 9.6 mmol) and acetic acid (0.15 ml, 2.6 mmol) were combined in methanol (100 ml). After 2.5 hours at room temperature, the reaction mixture was treated with additional formaldehyde (0.15 ml, 1.8 mmol) and allowed to stir for an additional 16 hours. The reaction was then filtered, and the filtrate was concentrated in vacuo and purified by column chromatography (eluant: 89:10:1 of chloroform:methanol:concentrated ammonium hydroxide), providing the title product as a white solid (1.04 g, 5.7 mmol).

후처리

  1. filtrationThe reaction was then filtered
  2. concentrationthe filtrate was concentrated in vacuo
  3. custompurified by column chromatography (eluant: 89:10:1 of chloroform:methanol:concentrated ammonium hydroxide)

출처 및 근거

ORD 기록
ord-cba5fcd9d46d46cdb9c7eca0684ae0fa
출처 데이터셋
uspto-grants-1993_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05214051

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