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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Dichloromethane → HCID 15409321, 화합물

HRID 1417955
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HRID 1417955 반응식
Cl[C:2]1[O:6][N:5]=[C:4]2[C:7]3[C:12]([CH2:13][CH2:14][C:3]=12)=[CH:11][CH:10]=[CH:9][CH:8]=3.[CH2:15]([N:22]1[CH2:27][CH2:26][NH:25][CH2:24][CH2:23]1)[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.C([O-])([O-])=O.[K+].[K+].C(Cl)Cl>CN1CCCC1=O.C(Cl)(Cl)Cl.CCOC(C)=O>[CH2:15]([N:22]1[CH2:27][CH2:26][N:25]([C:2]2[O:6][N:5]=[C:4]3[C:7]4[C:12]([CH2:13][CH2:14][C:3]=23)=[CH:11][CH:10]=[CH:9][CH:8]=4)[CH2:24][CH2:23]1)[C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 6344DichloromethaneHCID 11430Potassium CarbonateHCID 759941-BenzylpiperazineHCID 10987412Naphth[1,2-c]isoxazole, 3-chloro-4,5-dihydro-

생성물 1

HCID 15409321HCID 15409321, 화합물

시약·촉매·용매 3

HCID 6212Chloroform용매
HCID 8857
Ethyl Acetate
용매
HCID 13387N-methyl-2-pyrrolidone용매

실험 절차

A stirred mixture of 3-chloro-4,5-dihydronaphth[1,2-c]isoxazole (2.0 g, 9.75 mmol), 1-benzylpiperazine (17 ml, 97.5 mmol) and K2CO3 (2.7 g, 19.5 mmol) in 18 ml of N-methylpyrrolidinone under N2 was lowered into an oil bath preheated to 150° C. The mixture was heated while stirring under N2 for 2 hours. At that time, TLC (CH2Cl2) showed no remaining starting material. The mixture was removed from the heating bath, allowed to cool to room temperature and extracted with heptane. The organic phase was dried over MgSO4, filtered and concentrated in vacuo to obtain a crude solid. The solid was collected, titrated with Et2O, recrystallized from Et2O and dried in vacuo (0.1 mm) at 85° C. to provide pure product, mp of 164°-166° C., homogeneous by TLC [silica, 1:1 EtOAc, Rf=0.80]. The IR (CHCl3), NMR (CDCl3) and Mass Spectrum (M+ =345, EI, 70 eV) were consistent with the structure. The yield was 1.219 g (3.53 mmol, 36.24%).

후처리

  1. customwas lowered into an oil bath
  2. custompreheated to 150° C
  3. temperatureThe mixture was heated
  4. customThe mixture was removed from the heating bath
  5. extractionextracted with heptane
  6. dry with materialThe organic phase was dried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo
  9. customto obtain a crude solid
  10. customThe solid was collected
  11. customrecrystallized from Et2O
  12. customdried in vacuo (0.1 mm) at 85° C.
  13. customto provide pure product, mp of 164°-166° C.

출처 및 근거

ORD 기록
ord-5120a50d6ba44aaaaa1327dbc6f1b740
출처 데이터셋
uspto-grants-1999_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05880121

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