3-Methoxypropanehydrazide → HCID 178494843、化合物

HRID 541319ノート

反応式

HRID 541319 の反応式
C(S[N:4]=[CH:5][C:6]1[C:7]([CH:17]([CH3:19])[CH3:18])=[CH:8][C:9]([CH3:16])=[C:10]([CH:15]=1)[C:11]([O:13][CH3:14])=[O:12])C.[CH3:20][O:21][CH2:22][CH2:23][C:24]([NH:26][NH2:27])=O>C(O)(=O)C>[CH:17]([C:7]1[C:6]([C:5]2[NH:4][C:24]([CH2:23][CH2:22][O:21][CH3:20])=[N:26][N:27]=2)=[CH:15][C:10]([C:11]([O:13][CH3:14])=[O:12])=[C:9]([CH3:16])[CH:8]=1)([CH3:18])[CH3:19]

参加物

4

反応物 2

HCID 27597273-Methoxypropanehydrazide2 回HCID 86672536Methyl 5-((ethylthio)(imino)methyl)-4-isopropyl-2-methylbenzoate2 回

生成物 1

HCID 178494843HCID 178494843、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
80 °C

実験手順

Methyl 5-((ethylthio)(imino)methyl)-4-isopropyl-2-methylbenzoate (compound 198.4, 33 mg, 0.12 mmol, 1.0 equiv), 3-methoxypropanehydrazide (compound 143.1, 21 mg, 0.18 mmol, 1.5 equiv) and acetic acid (1.2 mL) were added to a 4-mL vial and heated at 80° C. with a loose cap for 4 hours. The solvent was removed in vacuo and the residue was dissolved in DCM (10 mL) and washed with saturated NaHCO3 (5 mL) then brine (5 mL), dried (Na2SO4), filtered and evaporated to a colorless oil (theoretical yield). m/z (ES+) 318 (M+H)+.

後処理

  1. customa loose cap for 4 hours
  2. customThe solvent was removed in vacuo
  3. dissolutionthe residue was dissolved in DCM (10 mL)
  4. washwashed with saturated NaHCO3 (5 mL)
  5. dry with materialbrine (5 mL), dried (Na2SO4)
  6. filtrationfiltered
  7. customevaporated to a colorless oil (theoretical yield)

出典と根拠

ORDレコード
ord-646c84b34c3042069b81d5fe9249e604
出典データセット
uspto-grants-2014_10
特許番号
US08871790B2

反応ノート

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