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Ammonia → n-(3-Oxopropyl)-n-phenethyl-3-phenethyloxy-propanamide

HRID 2234178
ノート
印刷プレビュー

反応式

HRID 2234178 の反応式
C([O:3][CH:4](OCC)[CH2:5][CH2:6][N:7]([CH2:21][CH2:22][C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)[C:8](=[O:20])[CH2:9][CH2:10][O:11][CH2:12][CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)C.Cl.Cl.NCCC1C2SC(=O)NC=2C(O)=CC=1.C([BH3-])#N.[Na+].N>O1CCOCC1.CO.O.C(O)(=O)C.ClCCl>[O:3]=[CH:4][CH2:5][CH2:6][N:7]([CH2:21][CH2:22][C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)[C:8](=[O:20])[CH2:9][CH2:10][O:11][CH2:12][CH2:13][C:14]1[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

11

反応物 5

HCID 222AmmoniaHCID 313Hydrochloric AcidHCID 5003444Sodium cyanoborohydrideHCID 602075534-Hydroxy-7-(2-aminoethyl)-1,3-benzothiazol-2(3H)-one hydrochlorideHCID 68701548N-(3,3-Diethoxypropyl)-N-phenethyl-3-phenethyloxy-propanamide

生成物 1

HCID 86258469n-(3-Oxopropyl)-n-phenethyl-3-phenethyloxy-propanamide

試薬・触媒・溶媒 5

HCID 176Acetic Acid溶媒HCID 887Methanol溶媒HCID 962Water溶媒HCID 6344Dichloromethane溶媒HCID 312751,4-Dioxane溶媒

実験手順

A solution of N-(3,3-diethoxypropyl)-N-phenethyl-3-phenethyloxy-propanamide (Example 8b), 0.127 g) in dioxane (10 mL) was treated with concentrated hydrochloric acid (1 mL) and stirred at room temperature for 30 minutes. After this time the solution was diluted (dichloromethane 30 mL), washed with water (2×20 mL), brine (20 mL), dried over magnesium sulfate and concentrated to give the crude aldehyde product (0.13 g) which was used immediately. The crude aldehyde was dissolved in methanol (20 mL) and 7-(2-aminoethyl)-4-hydroxy-3H-benzothiazol-2-one hydrochloride (0.078 g) was added along with acetic acid (0.1 mL) and water (0.1 mL). After stirring at room temperature for 30 minutes, sodium cyanoborohydride (0.012 g) was added and the reaction mixture stirred overnight. Ammonia (7N in methanol, 1 mL) was added and the mixture was concentrated. The resulting residue was taken up in ethyl acetate (50 mL), washed with water (2×20 mL), brine (20 mL), dried over magnesium sulfate and concentrated to give the crude product which was purified by flash column chromatography eluting with 1% ammonia; 5% methanol in dichloromethane to afford the titled compound as a white solid (0.078 g).

後処理

  1. washwashed with water (2×20 mL), brine (20 mL)
  2. dry with materialdried over magnesium sulfate
  3. concentrationconcentrated
  4. customto give the crude aldehyde product (0.13 g) which
  5. stirringAfter stirring at room temperature for 30 minutes
  6. stirringthe reaction mixture stirred overnight
  7. concentrationthe mixture was concentrated
  8. washwashed with water (2×20 mL), brine (20 mL)
  9. dry with materialdried over magnesium sulfate
  10. concentrationconcentrated
  11. customto give the crude product which
  12. customwas purified by flash column chromatography
  13. washeluting with 1% ammonia

出典と根拠

ORDレコード
ord-35be81b6fb14486eac53d0489883b7b6
出典データセット
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07709511B2

反応ノート

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