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Acetic Acid → 5-Chloro-6-methoxy-2,3-dihydrospiro[indene-1,3'-pyrrolidine]-2',5'-dione

HRID 1661057
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HRID 1661057 반응식
[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[O:11][CH3:12])[C:7]([CH2:15][C:16]#[N:17])([C:13]#N)[CH2:6][CH2:5]2.[OH2:18].CC(O)=[O:21]>OS(O)(=O)=O>[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[O:11][CH3:12])[C:7]1([CH2:15][C:16](=[O:18])[NH:17][C:13]1=[O:21])[CH2:6][CH2:5]2
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참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 962WaterHCID 674292935-chloro-1-(cyanomethyl)-6-methoxy-2,3-dihydro-1H-indene-1-carbonitrile

생성물 1

HCID 592339075-Chloro-6-methoxy-2,3-dihydrospiro[indene-1,3'-pyrrolidine]-2',5'-dione

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

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온도
200 °C

실험 절차

To a solution of 5-chloro-1-(cyanomethyl)-6-methoxy-2,3-dihydro-1H-indene-1-carbonitrile (Prep17, 520 mg, 2.11 mmol) in AcOH (5.2 ml), H2SO4 (0.364 ml) was added. The mixture was stirred for 15 min at 200° C. Water was added and the mixture extracted with EA twice, solvent was evaporated, dried over Na2SO4, concentrated to give the title compound that was used in the next step without further purification. (540 mg, y=96%).

후처리

  1. extractionthe mixture extracted with EA twice
  2. customsolvent was evaporated
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-f5f06d476696481f9c04a317d8e48c82
출처 데이터셋
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08030322B2

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