Acetic Acid → HCID 178451657、化合物

HRID 1713111ノート

反応式

HRID 1713111 の反応式
C[O-].[Na+].[CH:4]([NH2:6])=[NH:5].O=[C:8]1[CH2:14][CH2:13][N:12]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH2:11][CH2:10][CH:9]1[C:22](OC)=[O:23].C(O)(=O)C>CO>[OH:23][C:22]1[C:9]2[CH2:10][CH2:11][N:12]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH2:13][CH2:14][C:8]=2[N:6]=[CH:4][N:5]=1

参加物

6

反応物 4

HCID 176Acetic AcidHCID 68047FormamidineHCID 10942334Sodium MethoxideHCID 57479414HCID 57479414、化合物

生成物 1

HCID 178451657HCID 178451657、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

A solution of NaOMe in MeOH (13.6 mL, 25% in MeOH, 59.5 mmol) is added to a stirred solution of formamidine (2.2 g, 21 mmol) in MeOH (50 ml) at rt. The mixture is stirred for 15 min. 1-tert-Butyl 4-methyl 5-oxoazepane-1,4-dicarboxylate (5 g, 7.5 mmol) is added and the mixture is stirred at rt overnight. Acetic acid (2.33 g, 38.5 mmol) is added and the solvent is removed in vacuo. Water (30 ml) is added to the residue and the solution is extracted with DCM (3×30 ml). The combined extracts are washed with brine (40 ml), dried (Na2SO4) and evaporated, to provide a yellow solid that is used in the next step without further purification.

後処理

  1. stirringthe mixture is stirred at rt overnight
  2. customthe solvent is removed in vacuo
  3. additionWater (30 ml) is added to the residue
  4. extractionthe solution is extracted with DCM (3×30 ml)
  5. washThe combined extracts are washed with brine (40 ml)
  6. dry with materialdried (Na2SO4)
  7. customevaporated
  8. customto provide a yellow solid that
  9. customis used in the next step without further purification

出典と根拠

ORDレコード
ord-bbf2991210f548aa9c16d95d154514df
出典データセット
uspto-grants-2010_09
特許番号
US07795262B2

反応ノート

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