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2-Methylcinnamic aldehyde → HCID 53837773、化合物

HRID 1906397
ノート
印刷プレビュー

反応式

HRID 1906397 の反応式
C1(C)C=CC(S(O)(=O)=O)=CC=1.[CH2:12]([O:19][C:20]([CH2:22][CH2:23][CH2:24][CH2:25][NH2:26])=[O:21])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.[OH-].[Na+].[CH3:29][C:30](=[CH:33][C:34]1[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=1)[CH:31]=O.[BH4-].[Na+]>C(OCC)(=O)C.O.ClCCl>[CH2:12]([O:19][C:20]([CH2:22][CH2:23][CH2:24][CH2:25][NH:26][CH2:29][C:30]([CH3:31])=[CH:33][C:34]1[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=1)=[O:21])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH: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 75572-Methylcinnamic aldehydeHCID 14798Sodium HydroxideHCID 4311764Sodium borohydrideHCID 567770175-Aminopentanoic Acid Benzyl Ester Tosylate

生成物 1

HCID 53837773HCID 53837773、化合物収率 15%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane
溶媒
HCID 22728543Water ethylacetate溶媒

実験手順

13.7 g (36 mM) of 4-(benzyloxycarbonyl)butylamine para toluene sulphonate salt was stirred vigorously in ethyl acetate-water whilst being treated with aqueous sodium hydroxide to pH 9.5. The organic phase was washed with saturated brine, dried (anhydrous magnesium sulphate), benzyl alcohol (100 cm3) added, and the ethyl acetate evaporated. The solution was treated with one equivalent of α-methylcinnamaldehyde and stirred for 1/2 hour. Dichloromethane (50 cm3) was added and the reaction mixture treated with excess sodium borohydride. The mixture was filtered and the filtrate diluted with dichloromethane (100 cm3), washed with saturated brine (4×150 cm3) and dried (anhydrous magnesium sulphate). The dichloromethane was removed by evaporation under reduced pressure and the residue diluted with diethyl ether (300 cm3). This solution was treated with excess para toluene sulphonic acid in ether. The resultant crystals were filtered off, washed with ether and dried to yield 2.7 g (15%) of the title compound as a para-toluene sulphonate salt. This salt was extracted into ethyl acetate with aqueous sodium hydroxide (pH 9-10). The organic phase was washed with saturated brine, dried (anhydrous magnesium sulphate) and evaporated to an oil, yield=1.85 g (15%), (film) 3330, 1735, 1450, 1155, 750, 700 cm-1 ; (CDCl3) 1.35-2.00 (5H, m), 1.85 (3H, d, J 1 Hz), 2.37 and 2.62 (4H, 2 x t, J 6.5 Hz), 3.27 (2H, s), 5.10 (2H, s), 6.42 (1H, broad s), 7.26 and 7.34 (10H, 2×s).

後処理

  1. washThe organic phase was washed with saturated brine
  2. dry with materialdried (anhydrous magnesium sulphate), benzyl alcohol (100 cm3)
  3. additionadded
  4. customthe ethyl acetate evaporated
  5. filtrationThe mixture was filtered
  6. additionthe filtrate diluted with dichloromethane (100 cm3)
  7. washwashed with saturated brine (4×150 cm3)
  8. dry with materialdried (anhydrous magnesium sulphate)
  9. customThe dichloromethane was removed by evaporation under reduced pressure
  10. additionthe residue diluted with diethyl ether (300 cm3)
  11. additionThis solution was treated with excess para toluene sulphonic acid in ether
  12. filtrationThe resultant crystals were filtered off
  13. washwashed with ether
  14. customdried

出典と根拠

ORDレコード
ord-544d433151394831aa8ca7d140b6bfef
出典データセット
uspto-grants-1987_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04652560

反応ノート

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