Potassium Carbonate → 3-(2-Morpholinoethoxy)-1-(3,4,5-trimethoxyphenylacetyl) pyrrolidine Hemihydrate

HRID 839713

反応式

HRID 839713 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:13][C:14](Cl)=[O:15])[CH:6]=[C:7]([O:11][CH3:12])[C:8]=1[O:9][CH3:10].[O:17]1[CH2:22][CH2:21][N:20]([CH2:23][CH2:24][O:25][CH:26]2[CH2:30][CH2:29][NH:28][CH2:27]2)[CH2:19][CH2:18]1.C(=O)([O-])[O-].[K+].[K+]>C1C=CC=CC=1>[OH2:2].[O:17]1[CH2:18][CH2:19][N:20]([CH2:23][CH2:24][O:25][CH:26]2[CH2:30][CH2:29][N:28]([C:14](=[O:15])[CH2:13][C:5]3[CH:4]=[C:3]([O:2][CH3:1])[C:8]([O:9][CH3:10])=[C:7]([O:11][CH3:12])[CH:6]=3)[CH2:27]2)[CH2:21][CH2:22]1.[O:17]1[CH2:18][CH2:19][N:20]([CH2:23][CH2:24][O:25][CH:26]2[CH2:30][CH2:29][N:28]([C:14](=[O:15])[CH2:13][C:5]3[CH:4]=[C:3]([O:2][CH3:1])[C:8]([O:9][CH3:10])=[C:7]([O:11][CH3:12])[CH:6]=3)[CH2:27]2)[CH2:21][CH2:22]1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 110321242-(3,4,5-trimethoxyphenyl)acetyl ChlorideHCID 213331654-[2-(Pyrrolidin-3-yloxy)ethyl]morpholine

生成物 1

HCID 706050833-(2-Morpholinoethoxy)-1-(3,4,5-trimethoxyphenylacetyl) pyrrolidine Hemihydrate収率 70%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒2 回

実験手順

Under anhydrous conditions 5.3 g. crude 3,4,5-trimethoxyphenylacetic acid chloride [equivalent to 4.5 g. (0.0184 mole) by nuclear resonance spectrum analysis] in 20 ml. dry benzene was added dropwise to a stirring mixture of 3.7 g. (0.0184 mole) of 3-(2-morpholinoethoxy)pyrrolidine and 30 g. (0.0217 mole) of potassium carbonate in 50 ml. dry benzene. The product formed rapidly and separated out as a gummy mass. After stirring 1 hr. at room temperature, chloroform was stirred into the reaction mixture to dissolve the product. The inorganic materials were removed by filtration and the filtrate concentrated at reduced pressure to give 5.3 g. crude product (70% yield). A portion (2.6 g.) of the crude product was chromatographed on magnesium silicate to give 1.6 g. of pure product.

後処理

  1. customThe product formed rapidly
  2. customseparated out as a gummy mass
  3. stirringat room temperature, chloroform was stirred into the reaction mixture
  4. dissolutionto dissolve the product
  5. customThe inorganic materials were removed by filtration
  6. concentrationthe filtrate concentrated at reduced pressure
  7. customto give 5.3 g

出典と根拠

ORDレコード
ord-94936033071b4c399849ffb9e69a4733
出典データセット
uspto-grants-1978_06
特許番号
US04096331

関連ノート

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