Potassium Chloride → 6-Methyl-9-(2-hydroxyethyl)-1,2,3,4-tetrahydrocarbazol-1-one

HRID 127910

反応式

HRID 127910 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]2[C:12](=[CH:13][CH:14]=1)[NH:11][C:10]1[C:9](=[O:15])[CH2:8][CH2:7][CH2:6][C:5]2=1.CN(C)C=O.[Cl-].[K+].[CH2:23]1[O:25][CH2:24]1>O>[CH3:1][C:2]1[CH:3]=[C:4]2[C:12](=[CH:13][CH:14]=1)[N:11]([CH2:23][CH2:24][OH:25])[C:10]1[C:9](=[O:15])[CH2:8][CH2:7][CH2:6][C:5]2=1

参加物

6

反応物 4

HCID 4873Potassium ChlorideHCID 6228DimethylformamideHCID 6354Ethylene OxideHCID 6079846-methyl-2,3,4,9-tetrahydro-1H-carbazol-1-one

生成物 1

HCID 128776436-Methyl-9-(2-hydroxyethyl)-1,2,3,4-tetrahydrocarbazol-1-one

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
50 °C

実験手順

199 g. (1mole) of 6-methyl-1,2,3,4-tetrahydrocarbazol-1-one dissolved in 2000 ml. of dimethylformamide are taken initially and 5.6 g. (0.1 mole) of potassium chloride dissolved in 200 ml. of water are added. Thereafter 66.1 g.=74.2 ml. (1.5 mole) of ethyleneoxide are added at room temperature and heated up to 50° C. within 30 minutes, a maximum pressure of 0.2 to 0.5 bar being generated. Stirring is done for 20 hours at 50° C., the solvent is distilled off in a vacuum and, the residue is stirred with a mixture of 800 ml. water and 10 ml. of glacial acetic acid; the product (which takes a crystalline form) is filtered with suction, washed with 500 ml. water and dried at 40° C. in vacuo.

後処理

  1. distillationthe solvent is distilled off in a vacuum
  2. stirringthe residue is stirred with a mixture of 800 ml
  3. filtrationis filtered with suction
  4. washwashed with 500 ml
  5. dry with materialwater and dried at 40° C. in vacuo

出典と根拠

ORDレコード
ord-ebf3934fecc64e38a2233b2dfb44d7e7
出典データセット
uspto-grants-1981_03
特許番号
US04258043

関連ノート

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