Formaldehyde → HCID 19600144, 화합물

HRID 611213노트

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HRID 611213 반응식
[C:1]1([CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][S:12]([N:15]2[CH2:20][CH2:19][C:18]3[O:21][CH:22]=[CH:23][C:17]=3[CH2:16]2)(=[O:14])=[O:13])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH2:24]([NH:26][CH2:27][CH3:28])[CH3:25].[CH2:29]=O>C(O)(=O)C>[CH2:24]([N:26]([CH2:29][C:22]1[O:21][C:18]2[CH2:19][CH2:20][N:15]([S:12]([CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][C:1]3[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=3)(=[O:14])=[O:13])[CH2:16][C:17]=2[CH:23]=1)[CH2:27][CH3:28])[CH3:25]

참가 물질

5

반응물 3

HCID 712FormaldehydeHCID 8021DiethylamineHCID 19600103HCID 19600103, 화합물

생성물 1

HCID 19600144HCID 19600144, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

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온도
100 °C

실험 절차

To a solution of 0.269 g (0.807 mmol) of 5-(5-phenylpentylsulfonyl)-4,5,6,7-tetrahydrofuro[3,2-c]pyridine in 20 ml of acetic acid, 0.10 ml (0.97 mmol) of diethylamine and 79 mg (0.97 mmol) of 37% aqueous formaldehyde were added, followed by stirring at 100° C. for 30 minutes. 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 (ethyl acetate to ethyl acetate/methanol=9/1) 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 (ethyl acetate to ethyl acetate/methanol=9/1)

출처 및 근거

ORD 기록
ord-b1d4981efb5d457c97ab023daf3987d2
출처 데이터셋
uspto-grants-1999_12
특허 번호
US05998433

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