Triethylamine → Coumate

HRID 1613412ノート

反応式

HRID 1613412 の反応式
[OH:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6]([CH3:13])=[CH:7][C:8](=[O:12])[O:9]2)=[CH:4][CH:3]=1.[S:14](Cl)(=[O:17])(=[O:16])[NH2:15].C(N(CC)CC)C>C(#N)C>[CH3:13][C:6]1[C:5]2[CH:4]=[CH:3][C:2]([O:1][S:14](=[O:17])(=[O:16])[NH2:15])=[CH:11][C:10]=2[O:9][C:8](=[O:12])[CH:7]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 24499Chlorosulfamic acidHCID 52805674-Methylumbelliferone

生成物 1

HCID 9859866Coumate収率 41.1%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒2 回

実験手順

A slurry of 7-hydroxy-4-methylcoumarin (17.6 g, 0.10 mole) in acetonitrile (100 ml) was treated with a total of 84 ml of 3M sulfamoyl chloride (0.255 mole) in acetonitrile. The mixture was then treated dropwise with triethylamine (25.8 g, 0.255 mole). The reaction temperature was allowed to rise to 45° without any cooling. The mixture was stirred overnight at ambient temperature. The precipitate was collected, triturated with water, and dried in a vacuum oven at 70° C. for 15 hr to give 10.5 g (41%) of white powder, mp 161°-164° C.

後処理

  1. customto rise to 45° without any cooling
  2. customThe precipitate was collected
  3. customtriturated with water
  4. customdried in a vacuum oven at 70° C. for 15 hr

出典と根拠

ORDレコード
ord-487c7c590f4a4da1b6f4ce8bc5e0a585
出典データセット
uspto-grants-1993_03
特許番号
US05192785

反応ノート

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