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Dimethylformamide → HCID 20468178, 화합물

HRID 1903198
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HRID 1903198 반응식
CN(C)C=O.[CH2:6]([N:13]1[C:23]2[C:18](=[CH:19][C:20]([OH:24])=[CH:21][CH:22]=2)[CH2:17][CH2:16][C:14]1=[O:15])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.C([O-])([O-])=O.[K+].[K+].[CH2:31]([N:33]([CH2:41][CH:42]1[CH2:47][CH2:46][CH2:45][CH2:44][O:43]1)[C:34](=[O:40])[CH2:35][CH2:36][CH2:37][CH2:38]Cl)[CH3:32]>C(Cl)(Cl)Cl.CO>[CH2:6]([N:13]1[C:23]2[C:18](=[CH:19][C:20]([O:24][CH2:38][CH2:37][CH2:36][CH2:35][C:34]([N:33]([CH2:41][CH:42]3[CH2:47][CH2:46][CH2:45][CH2:44][O:43]3)[CH2:31][CH3:32])=[O:40])=[CH:21][CH:22]=2)[CH2:17][CH2:16][C:14]1=[O:15])[C:7]1[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 6228DimethylformamideHCID 11430Potassium CarbonateHCID 20468180HCID 20468180, 화합물HCID 54008488HCID 54008488, 화합물

생성물 1

HCID 20468178HCID 20468178, 화합물

시약·촉매·용매 2

HCID 887Methanol용매
HCID 6212
Chloroform
용매
2회

실험 절차

Into 50 ml of dimethylformamide were added 1.9 g of 1-benzyl-6-hydroxy-3,4-dihydrocarbostyril, 1.8 g of K2CO3 and 0.5 g of KI. The mixture was heated at 60°-70° C. under stirring, then 3.4 g of N-ethyl-N-(2-tetrahydropyranylmethyl)-5-chloropentanic acid amide was added dropwise gradually thereto. After the addition operation, the reaction mixture was further stirred at the same temperature for 4 hours. Then the solvent was removed by distillation and the residue thus obtained was dissolved in 200 ml of chloroform and the chloroform layer was washed with a diluted hydrochloric acid, 1% NaOH aqueous solution and water in this order, then dried with anhydrous sodium sulfate. The drying agent was removed by filtratoon, and the mother liquor was concentrated, then the residue thus obtained was treated by a silica-gel column chromatography [solvent used was a mixture of chloroform:methanol=20:1 (v/v)]. 0.6 Grams of 1-benzyl-6-{4-[N-(2-tetrahydropyranylmethyl)-N-ethylaminocarbonyl]butoxy}-3,4-dihydrocarbostyril was obtained as in the form of a colorless syrupy substance.

후처리

  1. temperatureThe mixture was heated at 60°-70° C.
  2. stirringAfter the addition operation, the reaction mixture was further stirred at the same temperature for 4 hours
  3. customThen the solvent was removed by distillation
  4. customthe residue thus obtained
  5. washthe chloroform layer was washed with a diluted hydrochloric acid, 1% NaOH aqueous solution and water in this order
  6. dry with materialdried with anhydrous sodium sulfate
  7. customThe drying agent was removed by filtratoon
  8. concentrationthe mother liquor was concentrated
  9. customthe residue thus obtained
  10. additionwas treated by a silica-gel column chromatography [solvent

출처 및 근거

ORD 기록
ord-9ef257de176646d09241f62e6b23a622
출처 데이터셋
uspto-grants-1984_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04435404

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