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Hydrochloric Acid → 1-Benzyl-4-(4-amino-phenyl)-pyrrolidine-3-carboxylic acid ethyl ester

HRID 1266464
ノート
印刷プレビュー

反応式

HRID 1266464 の反応式
[CH2:1]([O:3][C:4]([CH:6]1[CH:10]([C:11]2[CH:16]=[CH:15][C:14]([N+:17]([O-])=O)=[CH:13][CH:12]=2)[CH2:9][N:8]([CH2:20][C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[CH2:7]1)=[O:5])[CH3:2].[Sn].Cl.C(=O)([O-])[O-].[Na+].[Na+]>O.C(O)C>[CH2:1]([O:3][C:4]([CH:6]1[CH:10]([C:11]2[CH:12]=[CH:13][C:14]([NH2:17])=[CH:15][CH:16]=2)[CH2:9][N:8]([CH2:20][C:21]2[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=2)[CH2:7]1)=[O:5])[CH3:2]
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 313Hydrochloric AcidHCID 10340Sodium CarbonateHCID 4151186Ethyl 1-benzyl-4-(4-nitrophenyl)pyrrolidine-3-carboxylateHCID 5352426Tin atom

生成物 1

HCID 536986181-Benzyl-4-(4-amino-phenyl)-pyrrolidine-3-carboxylic acid ethyl ester収率 52.6%

試薬・触媒・溶媒 2

HCID 702
Ethanol
溶媒
HCID 962Water溶媒

実験手順

A mixture of 1-benzyl-4-(4-nitro-phenyl)-pyrrolidine-3-carboxylic acid ethyl ester (15 g, Reference Example 6), tin (25.12 g), hydrochloric acid (230 mL, 3M) and ethanol (230 mL) was heated at reflux temperature for 1 hour. After cooling to room temperature the pH of the mixture was adjusted to 9 by addition of solid sodium carbonate. The mixture was then diluted with water to give a final volume of 1000 mL and then filtered through a pad of celite. The clear filtrate was extracted twice with ethyl acetate (1000 mL). The combined extracts were dried over magnesium sulfate and then evaporated. The crude residue was subjected to chromatography using a Prochrom LC60 column, 40 cm silica bed, 20-45 μm, eluting with a mixture of cyclohexane and ethyl acetate (70:30, v/v) at 100 cm3/minute flow rate. The fractions containing the compound with RF=60/171 (thin layer chromatography plate ref. #05719, Merck KGaA, 64271 Darmstatd, Germany, cyclohexane:ethyl acetate, 70:30, v/v) were pooled and concentrated under reduced pressure (2.7 kPa) to give the title compound (7.22 g) as a yellow oil.

後処理

  1. temperaturewas heated
  2. temperatureat reflux temperature for 1 hour
  3. customto give a final volume of 1000 mL
  4. filtrationfiltered through a pad of celite
  5. extractionThe clear filtrate was extracted twice with ethyl acetate (1000 mL)
  6. dry with materialThe combined extracts were dried over magnesium sulfate
  7. customevaporated
  8. washeluting with a mixture of cyclohexane and ethyl acetate (70:30, v/v) at 100 cm3/minute flow rate
  9. additionThe fractions containing the compound with RF=60/171 (thin layer chromatography plate ref. #05719, Merck KGaA, 64271 Darmstatd, Germany, cyclohexane:ethyl acetate, 70:30, v/v)
  10. concentrationconcentrated under reduced pressure (2.7 kPa)

出典と根拠

ORDレコード
ord-b0cf331c5a944c518d18ab530e41578a
出典データセット
uspto-grants-2003_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06548533B2

反応ノート

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