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Triethylamine → HCID 20137301, 화합물

HRID 1253182
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HRID 1253182 반응식
[Cl:1][C:2]1[C:7]2[O:8][CH2:9][C:10](=[O:12])[NH:11][C:6]=2[N:5]=[C:4]([CH3:13])[N:3]=1.C(N(CC)CC)C.[CH2:21]([N:23]([CH2:27][CH3:28])[CH2:24][CH2:25][NH2:26])[CH3:22]>C1C=CC=CC=1>[ClH:1].[ClH:1].[CH2:21]([N:23]([CH2:27][CH3:28])[CH2:24][CH2:25][NH:26][C:2]1[C:7]2[O:8][CH2:9][C:10](=[O:12])[NH:11][C:6]=2[N:5]=[C:4]([CH3:13])[N:3]=1)[CH3:22]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 60993N,N-DiethylethylenediamineHCID 608089HCID 608089, 화합물

생성물 1

HCID 20137301HCID 20137301, 화합물수율 16%

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

A mixture containing 2 g of 4-chloro-2-methyl-6,7-dihydro-8H-pyrimido[5,4-b][1,4]oxazin-7-one, 1.52 g of triethylamine 1.16 g of 2-diethylaminoethylamine and 50 ml of abs. benzene is refluxed while stirring for 20 hours, then evaporated. After adding water to the residue, the pH is adjusted to 3 and the mixture is extracted with chloroform. The aqueous phase is alkalized to pH 9, extracted with chloroform, the latter organic phase is washed with water, dried and evaporated. The oily residue is taken up in ethanol and ethanolic hydrogen chloride solution is added. The precipitate is filtered to give 0.56 g (16%) of the product, m.p.: 252°-255° C.

후처리

  1. customevaporated
  2. additionAfter adding water to the residue
  3. extractionthe mixture is extracted with chloroform
  4. extractionextracted with chloroform
  5. washthe latter organic phase is washed with water
  6. customdried
  7. customevaporated
  8. additionethanolic hydrogen chloride solution is added
  9. filtrationThe precipitate is filtered

출처 및 근거

ORD 기록
ord-5111eb8ee3474911b63ac5ff8b1e9789
출처 데이터셋
uspto-grants-1988_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04748175

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