Water → HCID 19976898、化合物

HRID 1440320ノート

反応式

HRID 1440320 の反応式
[CH3:1][O:2][C:3]1[CH:12]=[CH:11][C:6]([C:7]([NH:9]Cl)=O)=[CH:5][CH:4]=1.[CH:13]#[C:14][CH:15]([OH:18])[CH2:16][CH3:17].C(N(CC)CC)C.[OH2:26]>C1C=CC=CC=1>[OH:18][CH:15]([C:16]1[O:26][N:9]=[C:7]([C:6]2[CH:11]=[CH:12][C:3]([O:2][CH3:1])=[CH:4][CH:5]=2)[CH:17]=1)[CH2:14][CH3:13]

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 929811-Pentyn-3-olHCID 21579386N-Chloro-4-methoxybenzamide

生成物 1

HCID 19976898HCID 19976898、化合物

試薬・触媒・溶媒 1

HCID 241Benzene溶媒2 回

実験手順

To a solution of 79.8 g (43 mmol) of 4-methoxybenzhydroxamic acid chloride and 7.23 g (86 mmol) of 1-pentyn-3-ol in 160 ml of benzene, a solution of 6.53 g (64.5 mmol) of triethylamine in 80 ml of benzene was added dropwise while maintaining the internal temperature at 3°-5° C. After the mixture was stirred for 2 hours, water was added so that the reaction product was extracted in the organic layer. The organic layer was separated and collected and the solvent was distilled off, whereby an oily residue was obtained. The oily residue was purified by silica gel chromatography (eluent: 30:1 chloroform/methyl alcohol), so that the title compound was obtained as yellow oil [yield: 8.07 g (81%)].

後処理

  1. temperaturewhile maintaining the internal temperature at 3°-5° C
  2. extractionwas extracted in the organic layer
  3. customThe organic layer was separated
  4. customcollected
  5. distillationthe solvent was distilled off
  6. customwhereby an oily residue was obtained
  7. customThe oily residue was purified by silica gel chromatography (eluent: 30:1 chloroform/methyl alcohol), so that the title compound
  8. customwas obtained as yellow oil [yield: 8.07 g (81%)]

出典と根拠

ORDレコード
ord-73a8b8638c4a4186938157a1a91bb58b
出典データセット
uspto-grants-1996_03
特許番号
US05498619

反応ノート

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