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Formaldehyde → Benzyl [3-methoxy-4-(1-methylpiperidin-4-yl)phenyl]carbamate

HRID 869254
ノート
印刷プレビュー

反応式

HRID 869254 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([NH:15][C:16](=[O:25])[O:17][CH2:18][C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[CH:6]=[CH:7][C:8]=1[CH:9]1[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]1.C=O.[C:28](O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C(=O)([O-])O.[Na+]>O.ClCCCl>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([NH:15][C:16](=[O:25])[O:17][CH2:18][C:19]2[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=2)[CH:6]=[CH:7][C:8]=1[CH:9]1[CH2:10][CH2:11][N:12]([CH3:28])[CH2:13][CH2:14]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 712FormaldehydeHCID 516892Sodium BicarbonateHCID 5049666Sodium triacetoxyborohydrideHCID 86662054Benzyl (3-methoxy-4-piperidin-4-ylphenyl)carbamate

生成物 1

HCID 86662055Benzyl [3-methoxy-4-(1-methylpiperidin-4-yl)phenyl]carbamate収率 79.6%

試薬・触媒・溶媒 2

HCID 11
1,2-Dichloroethane
溶媒
HCID 962Water溶媒

実験手順

To a mixture of benzyl (3-methoxy-4-piperidin-4-ylphenyl)carbamate (Preparation Example 455) (1.52 g) and 1,2-dichloroethane (70 mL), formalin (3.62 mL) and sodium triacetoxyborohydride (1.42 g) were added and stirred overnight at room temperature. After addition of water and saturated aqueous sodium hydrogen carbonate, the reaction liquid was extracted with chloroform, and the organic layer was dried over anhydrous magnesium sulfate. After the solvent was distilled off under reduced pressure, the residue was purified by silica gel column chromatography (eluent; chloroform:methanol:saturated aqueous ammonia=100:0:0 to 10:1:0.1) to give benzyl [3-methoxy-4-(1-methylpiperidin-4-yl)phenyl]carbamate (1.26 g) as a white solid.

後処理

  1. additionwere added
  2. customthe reaction liquid
  3. extractionwas extracted with chloroform
  4. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
  5. distillationAfter the solvent was distilled off under reduced pressure
  6. customthe residue was purified by silica gel column chromatography (eluent; chloroform:methanol:saturated aqueous ammonia=100:0:0 to 10:1:0.1)

出典と根拠

ORDレコード
ord-541203a8e55e4ecbb8cd6527c5d3dcd2
出典データセット
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08969336B2

反応ノート

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