Dimethylamine → HCID 23467112, 화합물

HRID 443385노트

반응식

HRID 443385 반응식
[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

참가 물질

5

반응물 3

HCID 674DimethylamineHCID 24614Phosphorus tribromideHCID 14567249HCID 14567249, 화합물

생성물 1

HCID 23467112HCID 23467112, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-2ab48a7df67248e08a4c8f832868e09a
출처 데이터셋
uspto-grants-1981_04
특허 번호
US04260611

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