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2-Chloro-N,N-dimethylethylamine → HCID 21873475, 화합물

HRID 723355
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HRID 723355 반응식
[H-].[Na+].[CH3:3][O:4][CH:5]([O:15][CH3:16])[CH2:6][NH:7][C:8]1[CH:13]=[CH:12][C:11]([OH:14])=[CH:10][CH:9]=1.[CH3:17][N:18]([CH3:22])[CH2:19][CH2:20]Cl>CN(C)C=O.C(OCC)(=O)C>[CH3:16][O:15][CH:5]([O:4][CH3:3])[CH2:6][NH:7][C:8]1[CH:13]=[CH:12][C:11]([O:14][CH2:20][CH2:19][N:18]([CH3:22])[CH3:17])=[CH:10][CH:9]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 79012-Chloro-N,N-dimethylethylamineHCID 24758Sodium hydrideHCID 21873414HCID 21873414, 화합물

생성물 1

HCID 21873475HCID 21873475, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

Sodium hydride (1.57 g) was added to a solution of 4-(2,2-dimethoxyethyl-amino)phenol (4.3 g) in dimethylformamide (25 mL). After 30 minutes, 2-dimethylaminoethyl chloride (hydrochloride, 3.14 g) was added. After 12 hours, the reaction solution was diluted with ethyl acetate and washed with water. The organic phase was dried and concentrated. The residue was purified by MPLC (eluent: dichloromethane/methanol/ammonia solution 95:4.9:0.1). The product with the molecular weight of 268.36 (C14H24N2O3); MS (ESI): 269 ([M+H]+), was obtained in this way.

후처리

  1. waitAfter 12 hours
  2. washwashed with water
  3. customThe organic phase was dried
  4. concentrationconcentrated
  5. customThe residue was purified by MPLC (eluent: dichloromethane/methanol/ammonia solution 95:4.9:0.1)
  6. customMS (ESI): 269 ([M+H]+), was obtained in this way

출처 및 근거

ORD 기록
ord-9b15dc935e9048bdbf41f30abf19b0ea
출처 데이터셋
uspto-grants-2006_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07141561B2

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