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Triethylamine → N-{3-hydroxy-6-(2-hydroxyethoxy)-2,4,5-trimethylbenzyl}-N-methyl-2-(4-hydroxy-2-isopropyl-5-methylphenoxy)ethylamine hydrochloride

HRID 55383
ノート
印刷プレビュー

反応式

HRID 55383 の反応式
C(N(CC)CC)C.Cl.[CH3:9][NH:10][CH2:11][CH2:12][O:13][C:14]1[CH:19]=[C:18]([CH3:20])[C:17]([OH:21])=[CH:16][C:15]=1[CH:22]([CH3:24])[CH3:23].[OH:25][C:26]1[C:27]([CH3:40])=[C:28]([C:31]([O:36][CH2:37][CH2:38][OH:39])=[C:32]([CH3:35])[C:33]=1[CH3:34])[CH2:29][Cl:30]>CN(C)C=O>[ClH:30].[OH:25][C:26]1[C:27]([CH3:40])=[C:28]([C:31]([O:36][CH2:37][CH2:38][OH:39])=[C:32]([CH3:35])[C:33]=1[CH3:34])[CH2:29][N:10]([CH2:11][CH2:12][O:13][C:14]1[CH:19]=[C:18]([CH3:20])[C:17]([OH:21])=[CH:16][C:15]=1[CH:22]([CH3:24])[CH3:23])[CH3:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 199577083-Hydroxy-6-(2-hydroxyethoxy)-2,4,5-trimethylbenzyl chlorideHCID 67726891N-methyl-2-(4-hydroxy-2-isopropyl-5-methylphenoxy)ethylamine hydrochloride

生成物 1

HCID 19957689N-{3-hydroxy-6-(2-hydroxyethoxy)-2,4,5-trimethylbenzyl}-N-methyl-2-(4-hydroxy-2-isopropyl-5-methylphenoxy)ethylamine hydrochloride収率 81.1%

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

Triethylamine (2.8 ml) was added dropwise to a solution of N-methyl-2-(4-hydroxy-2-isopropyl-5-methylphenoxy)ethylamine hydrochloride (2.60 g) and 3-hydroxy-6-(2-hydroxyethoxy)-2,4,5-trimethylbenzyl chloride (2.45 g) in N,N-dimethylformamide (20 ml), and the mixture was stirred at room temperature for 16 hours. After the completion of the reaction, the reaction mixture was poured on ice water and extracted with ethyl acetate. The extract was washed with water, dried and concentrated to give 3.8 g of a pale brown oil. The oil was dissolved in a small amount of methanol and conc. hydrochloric acid (1.2 ml) was added. The solvent was distilled off under reduced pressure and the residue was recrystallized from ethanol-diethyl ether to give 2.9 g of the title compound (colorless crystals).

後処理

  1. customAfter the completion of the reaction
  2. additionthe reaction mixture was poured on ice water
  3. extractionextracted with ethyl acetate
  4. washThe extract was washed with water
  5. customdried
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-1f8e8fd70ccd4e9f9a30c97dc3d5de11
出典データセット
uspto-grants-1997_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05624961

反応ノート

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