Isopropylamine → 1-Benzyloxy-4-[3-(1-methylethyl)aminopropoxy]benzene

HRID 2417983노트

반응식

HRID 2417983 반응식
[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([O:15][CH2:16][CH2:17][CH2:18]Br)=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH:20]([NH2:23])([CH3:22])[CH3:21]>>[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([O:15][CH2:16][CH2:17][CH2:18][NH:23][CH:20]([CH3:22])[CH3:21])=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

3

반응물 2

HCID 6363IsopropylamineHCID 111100311-(Benzyloxy)-4-(3-bromopropoxy)benzene

생성물 1

HCID 133384801-Benzyloxy-4-[3-(1-methylethyl)aminopropoxy]benzene

실험 절차

In a glass lined vessel, 1-benzyloxy-4-(3-bromopropoxy)benzene (33.4 g) in 300 ml of isopropylamine was heated at 100° for 10 hours under nitrogen at 1000 psi, then the excess isopropylamine was removed in vacuo and the residue was dissolved in 300 ml of water. The solution was made alkaline with 10% sodium hydroxide and the resulting oil extracted with dichloromethane. The dichloromethane extract, dried over potassium carbonate, was concentrated and distilled to yield 22.5 g of 1-benzyloxy-4-[3-(1-methylethyl)aminopropoxy]benzene, boiling range 180°-190° (0.5 mm) (97.8% pure by gas chromatography).

후처리

  1. customthe excess isopropylamine was removed in vacuo
  2. dissolutionthe residue was dissolved in 300 ml of water
  3. extractionthe resulting oil extracted with dichloromethane
  4. extractionThe dichloromethane extract
  5. dry with materialdried over potassium carbonate
  6. concentrationwas concentrated
  7. distillationdistilled

출처 및 근거

ORD 기록
ord-df6fbda604b34d58a22b9567905b59b2
출처 데이터셋
uspto-grants-1984_09
특허 번호
US04471116

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