Diisopropyl Ether → 2-[4-(Diethylamino)styryl]-5-ethyl-1-propylpyridinium bromide hemihydrate

HRID 365119

반응식

HRID 365119 반응식
[Br-:1].[CH2:2]([C:4]1[CH:5]=[CH:6][C:7]([CH3:13])=[N+:8]([CH2:10][CH2:11][CH3:12])[CH:9]=1)[CH3:3].[CH2:14]([N:16]([CH2:25][CH3:26])[C:17]1[CH:24]=[CH:23][C:20]([CH:21]=[O:22])=[CH:19][CH:18]=1)[CH3:15].N1CCCCC1.C(OC(C)C)(C)C>CO.C(O)(C)C.CCOCC>[OH2:22].[Br-:1].[CH2:25]([N:16]([CH2:14][CH3:15])[C:17]1[CH:24]=[CH:23][C:20]([CH:21]=[CH:13][C:7]2[CH:6]=[CH:5][C:4]([CH2:2][CH3:3])=[CH:9][N+:8]=2[CH2:10][CH2:11][CH3:12])=[CH:19][CH:18]=1)[CH3:26].[CH2:14]([N:16]([C:17]1[CH:18]=[CH:19][C:20]([CH:21]=[CH:13][C:7]2[CH:6]=[CH:5][C:4]([CH2:2][CH3:3])=[CH:9][N+:8]=2[CH2:10][CH2:11][CH3:12])=[CH:23][CH:24]=1)[CH2:25][CH3:26])[CH3:15].[Br-:1]

참가 물질

8

반응물 4

HCID 7914Diisopropyl EtherHCID 8082PiperidineHCID 671144-(Diethylamino)benzaldehydeHCID 133894285-Ethyl-2-methyl-1-propylpyridinium bromide

생성물 1

HCID 704551732-[4-(Diethylamino)styryl]-5-ethyl-1-propylpyridinium bromide hemihydrate수율 12.9%

시약·촉매·용매 3

HCID 887Methanol용매HCID 3283Diethyl Ether용매2회HCID 3776Isopropanol용매2회

실험 절차

5-Ethyl-2-methyl-1-propylpyridinium bromide (7.32 g, 0.03 mole) and 4-diethylaminobenzaldehyde (7.0 g, 0.04 mole) were refluxed for four hours in methanol (50 ml) in the presence of piperidine (1 ml) under nitrogen. On cooling and addition of ether no precipitate was obtained. The solution was evaporated to give a red oil which was dissolved in isopropanol and twice the volume of ether was added, when a red crystalline solid was obtained (5.4 g). 2 Grams were re-dissolved in isopropanol and isopropyl ether was added to give red crystals of 2-[4-(diethylamino)styryl]-5-ethyl-1-propylpyridinium bromide hemihydrate (1.6 g), melting point 165°-167° (decomposition).

후처리

  1. temperatureOn cooling
  2. customwas obtained
  3. customThe solution was evaporated
  4. customto give a red oil which
  5. customwhen a red crystalline solid was obtained (5.4 g)

출처 및 근거

ORD 기록
ord-cb54cf80e49b4a9f8b6db21eca512b2c
출처 데이터셋
uspto-grants-1986_08
특허 번호
US04608379

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