Water → 4-[(3-Benzyloxyphenyl)butylamino]-1-butanol

HRID 85327

反応式

HRID 85327 の反応式
[CH2:1]([O:8][C:9]1[CH:10]=[C:11](Br)[CH:12]=[CH:13][CH:14]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:16]([NH:20][CH2:21][CH2:22][CH2:23][CH2:24][OH:25])[CH2:17][CH2:18][CH3:19].C[Si](C)(C)[N-][Si](C)(C)C.[K+].O>O1CCOCC1.C(Cl)(Cl)Cl>[CH2:1]([O:8][C:9]1[CH:10]=[C:11]([CH2:19][CH2:18][CH2:17][CH2:16][NH:20][CH2:21][CH2:22][CH2:23][CH2:24][OH:25])[CH:12]=[CH:13][CH:14]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

7

反応物 4

HCID 962WaterHCID 206691-Butanol, 4-(butylamino)-HCID 27566381-(Benzyloxy)-3-bromobenzeneHCID 3251421Potassium bis(trimethylsilyl)amide

生成物 1

HCID 680090004-[(3-Benzyloxyphenyl)butylamino]-1-butanol収率 34.4%

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒HCID 312751,4-Dioxane溶媒

反応条件

温度
100 °C

実験手順

In 75 ml of dioxane were dissolved 5.19 g (19.7 mmol) of 3-benzyloxybromobenzene and 3.72 g (25.6 mmol) of 4-butylamino-1-butanol. To this mixture was added 5.89 g (29.5 mmol) of potassium hexamethyldisilazide and the mixture was stirred with heating at 100° C. for 22 hours. After the reaction mixture was poured into 200 ml of water, extraction with chloroform, washing with a saturated saline solution, drying over anhydrous sodium sulfate, and concentration were performed. The residue was purified by silica gel column chromatography to give 2.22 g of a light brown oily matter (yield: 34.4%).

後処理

  1. washwashing with a saturated saline solution
  2. dry with materialdrying over anhydrous sodium sulfate, and concentration
  3. customThe residue was purified by silica gel column chromatography
  4. customto give 2.22 g of a light brown oily matter (yield: 34.4%)

出典と根拠

ORDレコード
ord-c1da05f9c2d74ed5a63915189ce9ab7f
出典データセット
uspto-grants-2014_09
特許番号
US08846955B2

関連ノート

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