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Dichloromethane → HCID 15085583, 화합물

HRID 1607525
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HRID 1607525 반응식
[Na].[CH3:2][N:3]1[C:8](=[O:9])[C:7]2[S:10][CH:11]=[CH:12][C:6]=2[N:5]2[CH:13]=[N:14][C:15]([C:16]([O:18]CC)=O)=[C:4]12.[CH:21]1([C:24](=[N:26]O)[NH2:25])[CH2:23][CH2:22]1.C(Cl)Cl>C(O)C>[CH:21]1([C:24]2[N:26]=[C:16]([C:15]3[N:14]=[CH:13][N:5]4[C:6]5[CH:12]=[CH:11][S:10][C:7]=5[C:8](=[O:9])[N:3]([CH3:2])[C:4]=34)[O:18][N:25]=2)[CH2:23][CH2:22]1
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참가 물질

6

반응물 4

HCID 6344DichloromethaneHCID 2794666N'-HydroxycyclopropanecarboximidamideHCID 5360545SodiumHCID 15085587HCID 15085587, 화합물

생성물 1

HCID 15085583HCID 15085583, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Sodium (50 mg) was dissolved in dry ethanol (20 ml). Ethyl 4,5-dihydro-4-methyl-5-oxo-imidazo[1,5-a]thieno[2,3-e]-pyrimidine-3-carboxylate (0,55 g, 2 mmole), cyclopropanecarboxamide oxime (0,5 g, 5 mmole), and 5 g crushed mol. sieves 4 Å were added. The mixture was refluxed for 6 hours, then cooled to room temperature, where methylene chloride was added (30 ml). The mol. sieves were filtered off and the filtrate was reduced to 5 ml by evaporation in vacuo. Addition of water (25 ml) afforded a crystalline precipitate of the title compound which was collected by filtration. M.p. 215°-21° C. (Compound 8).

후처리

  1. additionsieves 4 Å were added
  2. temperatureThe mixture was refluxed for 6 hours
  3. filtrationsieves were filtered off
  4. customthe filtrate was reduced to 5 ml by evaporation in vacuo
  5. additionAddition of water (25 ml)

출처 및 근거

ORD 기록
ord-e8a816a4ddb743269c223f6441179018
출처 데이터셋
uspto-grants-1989_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04866065

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