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Acetic Acid → HCID 13257633, 화합물

HRID 647403
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HRID 647403 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:16](=[O:17])[C:15]3[CH2:14][CH2:13][CH2:12][CH2:11][C:10]=3[C:9]2=[O:18])=[C:4]([F:19])[CH:3]=1.[BH4-].[Na+].C(O)(=O)C>C(O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH:16]([OH:17])[C:15]3[CH2:14][CH2:13][CH2:12][CH2:11][C:10]=3[C:9]2=[O:18])=[C:4]([F:19])[CH:3]=1
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참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 1859312-(4-Chloro-2-fluorophenyl)-4,5,6,7-tetrahydro-1h-isoindole-1,3(2h)-dioneHCID 4311764Sodium borohydride

생성물 1

HCID 13257633HCID 13257633, 화합물수율 90%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

In 400 ml of ethanol was dissolved 40.0 g of 2-(4-chloro-2-fluorophenyl)-2,3,4,5,6,7-hexahydro-1H-isoindol-1,3-dione, and 2.4 g of sodium borohydride was added to the solution with stirring over a 30-minute period, while cooling was effected suitably to maintain the reaction temperature at 20° to 30° C. After stirring was continued at room temperature for one hour, the reaction mixture was neutralized with dilute acetic acid and concentrated to about one third of the original volume. Upon cooling, there resulted crystals, which were collected by filtration, washed with water and dried, thereby affording 36.2 g (yield of 90%) of the subject compound. Recrystallization from ethyl acetate yielded white crystals, m.p. 178°-179° C.

후처리

  1. additionwas added to the solution
  2. temperaturewhile cooling
  3. temperatureto maintain the reaction temperature at 20° to 30° C
  4. stirringAfter stirring
  5. concentrationconcentrated to about one third of the original volume
  6. temperatureUpon cooling
  7. customthere resulted crystals, which
  8. filtrationwere collected by filtration
  9. washwashed with water
  10. customdried

출처 및 근거

ORD 기록
ord-c35e4c79845c4ccbb76e9d7e609446bb
출처 데이터셋
uspto-grants-1983_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04409018

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