Dimethylamine → Ammonium Hydroxide

HRID 414478

반응식

HRID 414478 반응식
[CH:1]1[C:14]2[C:5](=[CH:6][C:7]3[C:12]([C:13]=2[O:15][CH2:16][CH2:17]Cl)=[CH:11][CH:10]=[CH:9][CH:8]=3)[CH:4]=[CH:3][CH:2]=1.[CH3:19][NH:20][CH3:21].O>C(O)O>[OH-:15].[NH4+:20].[CH:1]1[C:14]2[C:5](=[CH:6][C:7]3[C:12]([C:13]=2[O:15][CH2:16][CH2:17][N:20]([CH3:21])[CH3:19])=[CH:11][CH:10]=[CH:9][CH:8]=3)[CH:4]=[CH:3][CH:2]=1

참가 물질

6

반응물 3

HCID 674DimethylamineHCID 962WaterHCID 212808202-(9-Anthryloxy)ethyl chloride

생성물 2

HCID 14923Ammonium HydroxideHCID 143732391-(9-Anthryloxy)-2-dimethylaminoethane

시약·촉매·용매 1

HCID 79015Methanediol용매

실험 절차

2-(9-Anthryloxy)ethyl chloride (5.0 g) was heated for 5 hours at 90° C. in methylene glycol (50 ml) containing dimethylamine (4.0 g) using a dry ice condenser. The solution was cooled and added to water. The resulting mixture was extracted with ethyl acetate, and the extract dried and evaporated. The crude product was chromatographed on 100 g silica gel, eluting with a solution of methylene chloride:methanol:ammonium hydroxide, 95:5:1, to yield 1-(9-anthryloxy)-2-dimethylaminoethane, which was converted to the maleate, mp 132°-134° C.

후처리

  1. temperatureThe solution was cooled
  2. extractionThe resulting mixture was extracted with ethyl acetate
  3. customthe extract dried
  4. customevaporated
  5. customThe crude product was chromatographed on 100 g silica gel
  6. washeluting with a solution of methylene chloride

출처 및 근거

ORD 기록
ord-1e384aad5b3746e8bd63ec7d19772340
출처 데이터셋
uspto-grants-1988_12
특허 번호
US04792551

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