Benzaldehyde → HCID 14010268, 화합물

HRID 1731772노트

반응식

HRID 1731772 반응식
[ClH:1].[CH3:2][N:3]([CH3:11])[S:4]([NH:7][CH2:8][CH2:9][NH2:10])(=[O:6])=[O:5].[CH:12](=O)[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.C(N(CC)CC)C>C1C=CC=CC=1>[ClH:1].[CH:12](=[N:10][CH2:9][CH2:8][NH:7][S:4]([N:3]([CH3:11])[CH3:2])(=[O:6])=[O:5])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1

참가 물질

5

반응물 3

HCID 240BenzaldehydeHCID 8471TriethylamineHCID 14010266[(2-Aminoethyl)sulfamoyl]dimethylamine hydrochloride

생성물 1

HCID 14010268HCID 14010268, 화합물수율 50%

시약·촉매·용매 1

HCID 241Benzene용매2회

실험 절차

A mixture of 4.0 g (0.02 mole) of 2-[N-[(dimethylamino)sulfonyl]amino]ethylamine hydrochloride and 2.0 g (0.02 mole) of benzaldehyde was stirred and treated immediately with 2.0 g (0.02 mole) of triethylamine, followed by the addition of 200 ml of dry benzene. The solution was heated to reflux employing a Dean-Stark apparatus. After 2 hr at reflux, the benzene solution was cooled and washed twice with 100 ml portions of water. The organic phase was separated, dried over magnesium sulfate, and concentrated under reduced pressure to an oil, which was dissolved in ether and treated with HCl gas to precipitate a yellowish solid. The product was collected by filtration, washed with ether and air dried to provide 2.4 g (50%) of product. The NMR spectrum was consistent with the assigned structure and the solid was used without additional purification.

후처리

  1. temperatureThe solution was heated
  2. temperatureto reflux
  3. temperatureAfter 2 hr at reflux
  4. washwashed twice with 100 ml portions of water
  5. customThe organic phase was separated
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated under reduced pressure to an oil, which
  8. dissolutionwas dissolved in ether
  9. additiontreated with HCl gas
  10. customto precipitate a yellowish solid
  11. filtrationThe product was collected by filtration
  12. washwashed with ether and air
  13. customdried

출처 및 근거

ORD 기록
ord-5d7a066656ad4148b5dcf1a013b76652
출처 데이터셋
uspto-grants-1986_11
특허 번호
US04623652

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