Toluene → 2-(3-Morpholin-4-YL-propoxy)-benzaldehyde

HRID 26962

반응식

HRID 26962 반응식
[CH:1](=[O:9])[C:2]1[C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)[OH:4].[H-].[Na+].C1(C)C=CC=CC=1.Cl[CH2:20][CH2:21][CH2:22][N:23]1[CH2:28][CH2:27][O:26][CH2:25][CH2:24]1>CN(C)C=O.O>[N:23]1([CH2:22][CH2:21][CH2:20][O:4][C:3]2[CH:5]=[CH:6][CH:7]=[CH:8][C:2]=2[CH:1]=[O:9])[CH2:28][CH2:27][O:26][CH2:25][CH2:24]1

참가 물질

7

반응물 4

HCID 1140TolueneHCID 6998SalicylaldehydeHCID 24758Sodium hydrideHCID 958344-(3-Chloropropyl)morpholine

생성물 1

HCID 137952602-(3-Morpholin-4-YL-propoxy)-benzaldehyde

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

Salicylaldehyde (17 g) is treated first with 6.7 g of 50% sodium hydride in 110 ml of dimethylformamide and then with 92 ml of a 2 N toluene solution of N-(3-chloropropyl)morpholine. The mixture is heated at 105°-110° C. for 4 hours, cooled and poured into 300 ml of water. The product is extracted three times with ether. The extracts are combined, dried, concentrated on a rotary evaporator and the residue distilled to give 32.3 g of product as an oil, boiling point 155°-160° C. at 0.1-0.2 mm of Hg.

후처리

  1. temperatureThe mixture is heated at 105°-110° C. for 4 hours
  2. temperaturecooled
  3. extractionThe product is extracted three times with ether
  4. customdried
  5. concentrationconcentrated on a rotary evaporator
  6. distillationthe residue distilled

출처 및 근거

ORD 기록
ord-3813147e4d56433ea5d9617feb06058c
출처 데이터셋
uspto-grants-1979_04
특허 번호
US04151354

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