Dimethylamine → HCID 23467112、化合物

HRID 443385ノート

反応式

HRID 443385 の反応式
[Cl:1][C:2]1[N:3]=[C:4]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[C:5]2[C:10]([C:11]=1[CH2:12]O)=[CH:9][CH:8]=[CH:7][CH:6]=2.P(Br)(Br)Br.[CH3:24][NH:25][CH3:26]>C1(C)C=CC=CC=1>[Cl:1][C:2]1[N:3]=[C:4]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[C:5]2[C:10]([C:11]=1[CH2:12][N:25]([CH3:26])[CH3:24])=[CH:9][CH:8]=[CH:7][CH:6]=2

参加物

5

反応物 3

HCID 674DimethylamineHCID 24614Phosphorus tribromideHCID 14567249HCID 14567249、化合物

生成物 1

HCID 23467112HCID 23467112、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

8.2 g 3-Chloro-4-hydroxymethyl-1-phenyl-isoquinoline are suspended in 300 ml toluene and 16.2 g phosphorus tribromide are added thereto while cooling with ice. After a 10 hours' stirring at room temperature dimethylamine is introduced until an alcaline reaction occurs. The reaction mixture is concentrated and water is added to the residue. Extraction with acetic acid ester gives a yellow oil, that crystallizes slowly. Melting point 75° to 77° C. Hydrochloride: 244° to 246° C.

後処理

  1. temperaturewhile cooling with ice
  2. additionis introduced until an alcaline reaction
  3. concentrationThe reaction mixture is concentrated
  4. additionwater is added to the residue
  5. extractionExtraction with acetic acid ester
  6. customgives a yellow oil
  7. customthat crystallizes slowly
  8. custom244° to 246° C.

出典と根拠

ORDレコード
ord-2ab48a7df67248e08a4c8f832868e09a
出典データセット
uspto-grants-1981_04
特許番号
US04260611

反応ノート

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