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2-(2-(3-Methoxyphenyl)ethyl)phenol → 4-t-Butoxycarbonyl-2-{2-[2-(3-methoxyphenyl)ethyl]phenoxymethyl}morpholine

HRID 743259
ノート
印刷プレビュー

反応式

HRID 743259 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:9][CH2:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[OH:17])[CH:6]=[CH:7][CH:8]=1.[C:18]([O:22][C:23]([N:25]1[CH2:30][CH2:29][O:28][CH:27]([CH2:31]OS(C2C=CC(C)=CC=2)(=O)=O)[CH2:26]1)=[O:24])([CH3:21])([CH3:20])[CH3:19].CC(C)([O-])C.[K+]>CC(N(C)C)=O>[C:18]([O:22][C:23]([N:25]1[CH2:30][CH2:29][O:28][CH:27]([CH2:31][O:17][C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=2[CH2:10][CH2:9][C:5]2[CH:6]=[CH:7][CH:8]=[C:3]([O:2][CH3:1])[CH:4]=2)[CH2:26]1)=[O:24])([CH3:21])([CH3:19])[CH3:20]
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 105854482-(2-(3-Methoxyphenyl)ethyl)phenolHCID 19423893N-BOC-2-(tosyloxymethyl)morpholineHCID 23665647Potassium tert-butoxide

生成物 1

HCID 107173794-t-Butoxycarbonyl-2-{2-[2-(3-methoxyphenyl)ethyl]phenoxymethyl}morpholine収率 99.9%

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

実験手順

Following a procedure similar to that described in Example 40, 1.00 g of 2-[2-(3-methoxyphenyl)ethyl]phenol (prepared as described in Preparation 20), 1.63 g of 4-t-butoxycarbonyl-2-(p-toluenesulfonyloxymethyl)morpholine and 0.490 g of potassium t-butoxide were reacted in 20 ml of dimethylacetamide. The mixture was then worked up as described in Example 40, and the crude product thus obtained was purified by column chromatography through silica gel, using a 4:1 by volume mixture of hexane and ethyl acetate as the eluent, to give 1.87 g (yield 94.5%) of the title compound as a colorless oil.

後処理

  1. customthe crude product thus obtained
  2. customwas purified by column chromatography through silica gel
  3. additionby volume mixture of hexane and ethyl acetate as the eluent

出典と根拠

ORDレコード
ord-5d14d6df21654277b477188a471a393e
出典データセット
uspto-grants-1996_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05556864

反応ノート

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