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Water → 8-(2,4-Dichloro-5-methoxyphenyl)-1,4-dioxa-8-azaspiro[4.5]decane

HRID 1804855
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HRID 1804855 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:17][CH2:16][C:11]3([O:15][CH2:14][CH2:13][O:12]3)[CH2:10][CH2:9]2)=[CH:4][C:3]=1[O:18][CH3:19].[Cl:20]N1C(=O)CCC1=O.O.[OH-].[Na+]>CC(O)=O>[Cl:20][C:6]1[CH:7]=[C:2]([Cl:1])[C:3]([O:18][CH3:19])=[CH:4][C:5]=1[N:8]1[CH2:9][CH2:10][C:11]2([O:15][CH2:14][CH2:13][O:12]2)[CH2:16][CH2:17]1
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6

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HCID 962WaterHCID 14798Sodium HydroxideHCID 31398ChlorosuccinimideHCID 685538928-(4-Chloro-3-methoxyphenyl)-1,4-dioxa-8-azaspiro[4.5]decane

생성물 1

HCID 685558178-(2,4-Dichloro-5-methoxyphenyl)-1,4-dioxa-8-azaspiro[4.5]decane수율 91%

시약·촉매·용매 1

HCID 176
Acetic Acid
용매

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온도
60 °C

실험 절차

A mixture of 8-(4-chloro-3-methoxyphenyl)-1,4-dioxa-8-azaspiro[4.5]decane (1.67 g, 5.89 mmol, Example 13, step 1) and 1-chloropyrrolidine-2,5-dione (0.786 g, 5.89 mmol) in AcOH (15 mL) was heated at 60° C. overnight. The mixture was cooled and water was added. Upon completion of addition, the mixture was neutralized with 1N NaOH, extracted with EtOAc, dried (Na2SO4), and concentrated to give 8-(2,4-dichloro-5-methoxyphenyl)-1,4-dioxa-8-azaspiro[4.5]decane (1.7 g, 5.34 mmol, 91% yield) as a yellow oil.

후처리

  1. temperatureThe mixture was cooled
  2. additionUpon completion of addition
  3. extractionextracted with EtOAc
  4. dry with materialdried (Na2SO4)
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-ed24750daf544ffb9e95d1ba6049f47c
출처 데이터셋
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08354432B2

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