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

HRID 1390626노트

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HRID 1390626 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 241Benzene용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-384463053c1d43448333acbaf50ce46b
출처 데이터셋
uspto-grants-1979_02
특허 번호
US04139620

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