Phenol → N-butyl-N-(3-phenoxypropyl)butan-1-amine

HRID 1855320

반응식

HRID 1855320 반응식
[C:1]1([OH:7])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[OH-].[Na+].Cl.Cl[CH2:12][CH2:13][CH2:14][N:15]([CH2:20][CH2:21][CH2:22][CH3:23])[CH2:16][CH2:17][CH2:18][CH3:19]>O>[CH2:20]([N:15]([CH2:16][CH2:17][CH2:18][CH3:19])[CH2:14][CH2:13][CH2:12][O:7][C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1)[CH2:21][CH2:22][CH3:23]

참가 물질

5

반응물 3

HCID 996PhenolHCID 14798Sodium HydroxideHCID 225950531-Dibutylamino-3-chloropropane hydrochloride

생성물 1

HCID 5262101N-butyl-N-(3-phenoxypropyl)butan-1-amine수율 91.4%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

The process is performed in the same manner as previously (Example 13), starting with 138 g (1.466 mol; 1.15 eq.) of phenol, 109.5 g (2.738 mol; 2.15 eq.) of NaOH, 530 ml of distilled water and 308.9 g (1.275 mol; 1 eq.) of N-(3-chloropropyl)-N,N-dibutylamine hydrochloride. The mixture is refluxed for 16 hours. The oil formed is separated out by settling and washed with 500 ml of water and then diluted with 500 ml of MTBE and washed with 500 ml of 2% HCl. The MTBE phase is concentrated under vacuum and the oil is dried by azeotropic distillation with DCM. 307.1 g of the crude derivative N,N-dibutyl-N-(3-phenoxypropyl)amine are obtained.

후처리

  1. temperatureThe mixture is refluxed for 16 hours
  2. customThe oil formed
  3. customis separated out
  4. washwashed with 500 ml of water
  5. additiondiluted with 500 ml of MTBE
  6. washwashed with 500 ml of 2% HCl
  7. concentrationThe MTBE phase is concentrated under vacuum
  8. dry with materialthe oil is dried by azeotropic distillation with DCM

출처 및 근거

ORD 기록
ord-cededdaf22534e1cb4d123dcd746a4ca
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08962869B2

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