Dimethylacetamide → HCID 178457241、化合物

HRID 25536

反応式

HRID 25536 の反応式
[C:1]([O:5][C:6](=[O:21])[N:7]([C@H:9]1[CH2:14][CH2:13][C@H:12]([O:15][CH2:16][CH2:17][CH2:18][CH2:19]Br)[CH2:11][CH2:10]1)[CH3:8])([CH3:4])([CH3:3])[CH3:2].[CH2:22]([CH2:25][NH2:26])[CH:23]=C.[CH3:27]C(N(C)C)=O>>[C:1]([O:5][C:6](=[O:21])[N:7]([C@H:9]1[CH2:14][CH2:13][C@H:12]([O:15][CH2:16][CH2:17][CH2:18][CH2:19][N:26]([CH2:25][CH:22]=[CH2:23])[CH3:27])[CH2:11][CH2:10]1)[CH3:8])([CH3:4])([CH3:3])[CH3:2]

参加物

4

反応物 3

HCID 31374DimethylacetamideHCID 4437323-Buten-1-amineHCID 178486057HCID 178486057、化合物

生成物 1

HCID 178457241HCID 178457241、化合物収率 92%

実験手順

To 1.7 g (4.7 mmol) trans-[4-(4-Bromo-butoxy)-cyclohexyl]-methyl-carbamic acid tert-butyl ester in 22 ml DMA, 1.34 ml (14 mmol, 3 eq) N-allylmethylamine were added over a period of 10 min. The reaction was stirred at RT over night, concentrated and the residue was dissolved in CH2Cl2/5% aqueous NaHCO3. The phases were separated and the inorganic phase was extracted with CH2Cl2, the combined organic phases were washed with brine, dried over Na2SO4 and concentrated to yield 1.5 g (92%) trans-(4-[4-(Allyl-methyl-amino)-butoxy]-cyclohexyl)-methyl-carbamic acid tert-butyl ester as colorless oil, MS: 355 (MH+).

後処理

  1. concentrationconcentrated
  2. dissolutionthe residue was dissolved in CH2Cl2/5% aqueous NaHCO3
  3. customThe phases were separated
  4. extractionthe inorganic phase was extracted with CH2Cl2
  5. washthe combined organic phases were washed with brine
  6. dry with materialdried over Na2SO4
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-4128066c2cac404680c12d215436bd84
出典データセット
uspto-grants-2005_02
特許番号
US06858651B2

関連ノート

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