Dimethylamine → Ammonium Hydroxide

HRID 414478

反応式

HRID 414478 の反応式
[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

参加物

6

反応物 3

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

生成物 2

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

試薬・触媒・溶媒 1

HCID 79015Methanediol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1e384aad5b3746e8bd63ec7d19772340
出典データセット
uspto-grants-1988_12
特許番号
US04792551

関連ノート

読み込み中…