1-Chloro-2-(diethylamine)ethane hydrochloride → 27591-69-1

HRID 268515

반응식

HRID 268515 반응식
[CH2:1]([N:3]([CH2:7][CH3:8])[CH2:4][CH2:5][Cl:6])[CH3:2].Cl.[CH2:10]([N:12]([CH2:16][CH3:17])[CH2:13][CH2:14][Cl:15])[CH3:11].[OH:18][C:19]1[CH:31]=[CH:30][C:29]2[C:28]3[C:23](=[CH:24][C:25]([OH:32])=[CH:26][CH:27]=3)[C:22](=[O:33])[C:21]=2[CH:20]=1.C[O-].[Na+]>C1(C)C=CC=CC=1>[ClH:6].[ClH:15].[CH2:1]([N:3]([CH2:7][CH3:8])[CH2:4][CH2:5][O:18][C:19]1[CH:31]=[CH:30][C:29]2[C:28]3[C:23](=[CH:24][C:25]([O:32][CH2:14][CH2:13][N:12]([CH2:10][CH3:11])[CH2:16][CH3:17])=[CH:26][CH:27]=3)[C:22](=[O:33])[C:21]=2[CH:20]=1)[CH3:2]

참가 물질

6

반응물 4

HCID 133631-Chloro-2-(diethylamine)ethane hydrochlorideHCID 13364Diethylaminoethyl chlorideHCID 43541812,7-Dihydroxyfluoren-9-oneHCID 10942334Sodium Methoxide

생성물 1

HCID 3395827591-69-1

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

A solution of 2-diethylaminoethyl chloride [obtained from 15.5 g (0.09 mole) of 2-diethylaminoethyl chloride hydrochloride] in 100 ml of toluene (dried over molecular sieves) is added to a mixture of 6.4 g (0.03 mole) of 2,7-dihydroxyfluoren-9-one and 3.3 g (0.06 mole) of sodium methoxide in 200 ml of toluene (dried over molecular sieves). This mixture is heated to reflux with stirring for three hours. Upon cooling, the mixture is filtered to remove the precipitated sodium chloride. The toluene solution is washed three times with water, then once with a saturated sodium chloride solution and dried over anhydrous magnesium sulfate. This mixture is filtered, and the filtrate acidified to Congo Red with ethereal hydrogen chloride. The solid which precipitates is filtered, recrystallized from butanone with enough methanol added to effect solution, and the product dried at 100°C for 24 hours under vacuum to give 2,7-bis(2-diethylaminoethoxy)fluoren-9-one dihydrochloride. M.P. 235°-237°C.

후처리

  1. temperatureThis mixture is heated
  2. temperatureto reflux
  3. temperatureUpon cooling
  4. filtrationthe mixture is filtered
  5. customto remove the precipitated sodium chloride
  6. washThe toluene solution is washed three times with water
  7. dry with materialonce with a saturated sodium chloride solution and dried over anhydrous magnesium sulfate
  8. filtrationThis mixture is filtered
  9. customThe solid which precipitates
  10. filtrationis filtered
  11. customrecrystallized from butanone with enough methanol
  12. additionadded to effect solution
  13. customthe product dried at 100°C for 24 hours under vacuum

출처 및 근거

ORD 기록
ord-6729bfab90714f11b7329e58eae13f67
출처 데이터셋
uspto-grants-1976_03
특허 번호
US03947593

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