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Dichloromethane → HCID 18796731, 화합물

HRID 1003511
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HRID 1003511 반응식
C([O:3][C:4]([C:6]1[N:15]=[C:14]([NH:16][CH2:17][C:18]2[CH:23]=[CH:22][C:21]3[O:24][CH2:25][O:26][C:20]=3[CH:19]=2)[C:13]2[C:8](=[CH:9][CH:10]=[C:11]([Cl:27])[CH:12]=2)[N:7]=1)=O)C.C(Cl)Cl.O1CCCC1.[H-].C([Al+]CC(C)C)C(C)C>C1(C)C=CC=CC=1.CO>[CH:4]([C:6]1[N:15]=[C:14]([NH:16][CH2:17][C:18]2[CH:23]=[CH:22][C:21]3[O:24][CH2:25][O:26][C:20]=3[CH:19]=2)[C:13]2[C:8](=[CH:9][CH:10]=[C:11]([Cl:27])[CH:12]=2)[N:7]=1)=[O:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 6344DichloromethaneHCID 8028TetrahydrofuranHCID 18796730HCID 18796730, 화합물HCID 21225700Diisobutylaluminumhydride

생성물 1

HCID 18796731HCID 18796731, 화합물수율 52%

시약·촉매·용매 2

HCID 887Methanol용매
HCID 1140
Toluene
용매

실험 절차

0.50 g (0.0013 mol) of 2-ethoxycarbonyl-4-(3,4-methylenedioxybenzyl)amino-6-chloroquinazoline was dissolved in a solvent mixture comprising 20 ml of methylene chloride and 20 ml of tetrahydrofuran, 2.6 ml of a 1.0 M solution of diisobutylaluminum hydride in toluene was dropped into the solution prepared above at -78° C. under stirring. The obtained mixture was stirred at -78° C. for several hours, followed by the addition of 20 ml of methanol. The obtained mixture was distilled under a reduced pressure to remove the solvent. The residue was purified by silica gel column chromatography and recrystallized from ethyl acetate/n-hexane to give 0.23 g of the title compound as a pale-yellow crystal.

후처리

  1. additionwas dropped into the solution
  2. customprepared above at -78° C.
  3. stirringThe obtained mixture was stirred at -78° C. for several hours
  4. distillationThe obtained mixture was distilled under a reduced pressure
  5. customto remove the solvent
  6. customThe residue was purified by silica gel column chromatography
  7. customrecrystallized from ethyl acetate/n-hexane

출처 및 근거

ORD 기록
ord-0d860321923b460fb073db1020bb47a7
출처 데이터셋
uspto-grants-2000_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06046206

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