Methyl iodide → HCID 69707075、化合物

HRID 345811ノート

反応式

HRID 345811 の反応式
[CH2:1]([N:8]1[CH2:12][C@@H:11]([OH:13])[C@H:10]([NH:14][CH2:15][CH2:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H-].[Na+].[H][H].[CH3:27]I>O1CCCC1>[CH2:1]([N:8]1[CH2:12][C@@H:11]([O:13][CH3:27])[C@H:10]([NH:14][CH2:15][CH2:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH2:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

6

反応物 4

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 69706831trans-1-Benzyl-3-benzylmethylamino-4-hydroxypyrrolidineHCID 178418361HCID 178418361、化合物

生成物 1

HCID 69707075HCID 69707075、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

17.3 g (58 mmol) of crude trans-1-benzyl-3-benzylmethylamino-4-hydroxy-pyrrolidine in 80 ml of absolute tetrahydrofuran are added dropwise to 2.8 g (93.3 mmol) of 80% strength sodium hydride in 40 ml of absolute tetrahydrofuran and the mixture is heated under reflux at the same time. When the evolution of hydrogen has ended, 8.7 g (61 mmol) of methyl iodide are added dropwise and the mixture is then heated under reflux overnight. It is poured into ice-water and extracted with toluene, the extracts are dried with K2CO3 and concentrated and the residue is distilled.

後処理

  1. temperaturethe mixture is heated
  2. temperatureunder reflux at the same time
  3. temperaturethe mixture is then heated
  4. temperatureunder reflux overnight
  5. extractionextracted with toluene
  6. dry with materialthe extracts are dried with K2CO3
  7. concentrationconcentrated
  8. distillationthe residue is distilled

出典と根拠

ORDレコード
ord-fe6b6cd758c242288ed427d50ddacd91
出典データセット
uspto-grants-1991_10
特許番号
US05059597

反応ノート

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