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Hydrochloric Acid → HCID 67456106、化合物

HRID 242279
ノート
印刷プレビュー

反応式

HRID 242279 の反応式
C([O:3][C:4](=O)[C:5]([N:21]1[CH:25]=[CH:24][N:23]=[N:22]1)=[CH:6][NH:7][NH:8][C:9]1[CH:14]=[C:13]([N:15]2[CH2:20][CH2:19][O:18][CH2:17][CH2:16]2)[N:12]=[CH:11][N:10]=1)C.C[O-].[Na+].[ClH:30]>C(O)C.CO>[ClH:30].[N:15]1([C:13]2[N:12]=[CH:11][N:10]=[C:9]([N:8]3[C:4](=[O:3])[C:5]([N:21]4[CH:25]=[CH:24][N:23]=[N:22]4)=[CH:6][NH:7]3)[CH:14]=2)[CH2:20][CH2:19][O:18][CH2:17][CH2:16]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 10942334Sodium MethoxideHCID 674548403-[2-(6-morpholin-4-ylpyrimidin-4-yl)hydrazino]-2-(1H-1,2,3-triazol-1-yl)prop-2-enoic acid ethyl ester

生成物 1

HCID 67456106HCID 67456106、化合物

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 887Methanol
溶媒

反応条件

温度
10 °C

実験手順

Batch 2: A further amount of the title compound is obtained as follows: The residue (2.4 g) obtained from the mother liquor during the synthesis of Example Compound 71, which contains the open-ring intermediate state of the cyclization, 3-[2-(6-morpholin-4-ylpyrimidin-4-yl)hydrazino]-2-(1H-1,2,3-triazol-1-yl)prop-2-enoic acid ethyl ester, is dissolved in 12 ml ethanol and 1.5 ml 30% strength sodium methylate solution in methanol are added at RT, while stirring. The mixture is subsequently stirred at RT for 45 min, then adjusted to pH 5 with 2 N hydrochloric acid and subsequently stirred at RT for a further 16 h. The mixture is cooled to 10° C. and the solid is filtered off and washed with 3.5 ml dioxane. The mixture is dried under a high vacuum for 16 h, 5 ml methanol are then added and the mixture is subsequently stirred at RT for 1 h. The solid is filtered off, washed with 2 ml methanol and dried under a high vacuum to give a further 997 mg of the title compound in this way.

後処理

  1. stirringThe mixture is subsequently stirred at RT for 45 min
  2. stirringsubsequently stirred at RT for a further 16 h
  3. filtrationthe solid is filtered off
  4. washwashed with 3.5 ml dioxane
  5. customThe mixture is dried under a high vacuum for 16 h
  6. addition5 ml methanol are then added
  7. stirringthe mixture is subsequently stirred at RT for 1 h
  8. filtrationThe solid is filtered off
  9. washwashed with 2 ml methanol
  10. customdried under a high vacuum

出典と根拠

ORDレコード
ord-e4983f4e050646eeb65243067b169c2f
出典データセット
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08653111B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート