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Chloroform → tert-Butyl 2-[3-(N-Cyclohexylaminocarbonylmethyl)phenoxy]-2-methylpropionate

HRID 480688
ノート
印刷プレビュー

反応式

HRID 480688 の反応式
[C:1]([O:5][C:6]([C:8]([CH3:21])([O:10][C:11]1[CH:12]=[C:13]([CH2:17][C:18]([OH:20])=O)[CH:14]=[CH:15][CH:16]=1)[CH3:9])=[O:7])([CH3:4])([CH3:3])[CH3:2].C(Cl)(=O)C(Cl)=O.[CH:28]1([NH2:34])[CH2:33][CH2:32][CH2:31][CH2:30][CH2:29]1.C(Cl)(Cl)Cl>ClCCl>[CH:28]1([NH:34][C:18]([CH2:17][C:13]2[CH:12]=[C:11]([CH:16]=[CH:15][CH:14]=2)[O:10][C:8]([CH3:9])([CH3:21])[C:6]([O:5][C:1]([CH3:2])([CH3:3])[CH3:4])=[O:7])=[O:20])[CH2:33][CH2:32][CH2:31][CH2:30][CH2:29]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6212ChloroformHCID 7965CyclohexylamineHCID 65578Oxalyl chlorideHCID 187664143-(1-tert-Butoxycarbonyl-1-methylethoxy)phenylacetic Acid

生成物 1

HCID 18766566tert-Butyl 2-[3-(N-Cyclohexylaminocarbonylmethyl)phenoxy]-2-methylpropionate

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒

実験手順

3-(1-tert-Butoxycarbonyl-1-methylethoxy)phenylacetic acid (250 mg, 0.849 mmol) was dissolved in solvent mixture of dimethylformamide (10 μL)-dichloromethane (6 mL). Subsequently, oxalyl chloride [(COCl)2 (148 μL, 1.70 mmol)] was added at 0° C., the mixture was stirred for one hour at room temperature. The reaction mixture was added to a solution obtained by dissolving cyclohexylamine (0.97 mL, 8.49 mmol) in dichloromethane (1 mL) at 0° C., the mixture was stirred for one hour at room temperature. Chloroform was added to the reaction mixture. Washing was performed sequentially with 1M hydrochloric acid, water, and saturated brine, followed by drying over sodium sulfate. The mixture was subjected to concentration under reduced pressure and purification by silica gel column chromatography (chloroform/methanol=50/1), whereby the target compound was obtained (280 mg, 0.746 mmol, 87.8%).

後処理

  1. additionThe reaction mixture was added to a solution
  2. customobtained
  3. stirringthe mixture was stirred for one hour at room temperature
  4. washWashing
  5. dry with materialby drying over sodium sulfate
  6. concentrationThe mixture was subjected to concentration under reduced pressure and purification by silica gel column chromatography (chloroform/methanol=50/1), whereby the target compound
  7. customwas obtained (280 mg, 0.746 mmol, 87.8%)

出典と根拠

ORDレコード
ord-6e3d8b7d82454c8fab97b872deaf0c65
出典データセット
uspto-grants-2003_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06653334B1

反応ノート

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