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Formaldehyde → HCID 19600068, 화합물

HRID 611217
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HRID 611217 반응식
C(O[C:6]([N:8]([CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)[CH2:9][CH2:10][CH2:11][C:12]1[CH:16]=[CH:15][O:14][CH:13]=1)=O)(C)(C)C.C=O>C(O)(=O)C>[C:23]1([CH2:22][CH2:21][CH2:20][CH2:19][CH2:18][CH2:17][N:8]2[CH2:9][CH2:10][CH2:11][C:12]3[CH:16]=[CH:15][O:14][C:13]=3[CH2:6]2)[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1
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참가 물질

4

반응물 2

HCID 712FormaldehydeHCID 19600203HCID 19600203, 화합물

생성물 1

HCID 19600068HCID 19600068, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

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온도
100 °C

실험 절차

To a solution of the above crude N-[3-(3-furyl)propyl]-6-phenylhexylamine in 100 ml of acetic acid, 0.74 g (9.1 mmol) of 37% aqueous formaldehyde was added, followed by stirring at 100° C. for 1 hour. After the solvent was distilled off under reduced pressure, the residual solution was alkalified with aqueous sodium hydroxide and extracted with dichloromethane 3 times. The combined organic layer was dried over anhydrous magnesium sulfate; the solvent was distilled off under reduced pressure. The resulting crude product was purified by silica gel column chromatography (hexane/ethyl acetate=9/1 to 3/1) to yield the desired product.

후처리

  1. distillationAfter the solvent was distilled off under reduced pressure
  2. extractionextracted with dichloromethane 3 times
  3. dry with materialThe combined organic layer was dried over anhydrous magnesium sulfate
  4. distillationthe solvent was distilled off under reduced pressure
  5. customThe resulting crude product was purified by silica gel column chromatography (hexane/ethyl acetate=9/1 to 3/1)

출처 및 근거

ORD 기록
ord-78f390fdd6754aaa82d6dc2a943939a5
출처 데이터셋
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05998433

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