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Triethylamine → HCID 20137301、化合物

HRID 1253182
ノート
印刷プレビュー

反応式

HRID 1253182 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 60993N,N-DiethylethylenediamineHCID 608089HCID 608089、化合物

生成物 1

HCID 20137301HCID 20137301、化合物収率 16%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5111eb8ee3474911b63ac5ff8b1e9789
出典データセット
uspto-grants-1988_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04748175

反応ノート

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