N-Carbethoxyphthalimide → HCID 1548084、化合物

HRID 1531537ノート

反応式

HRID 1531537 の反応式
Cl.[CH2:2]([O:9][C:10]1[CH:21]=[C:20]2[C:13]([NH:14][CH:15]=[C:16]2[CH2:17][CH2:18][NH2:19])=[CH:12][CH:11]=1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.C(N1[C:31](=[O:32])[C:30]2=[CH:33][CH:34]=[CH:35][CH:36]=[C:29]2[C:28]1=[O:37])(OCC)=O>C(N(CC)CC)C>[CH2:2]([O:9][C:10]1[CH:21]=[C:20]2[C:13](=[CH:12][CH:11]=1)[NH:14][CH:15]=[C:16]2[CH2:17][CH2:18][N:19]1[C:31](=[O:32])[C:30]2[C:29](=[CH:36][CH:35]=[CH:34][CH:33]=2)[C:28]1=[O:37])[C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=1

参加物

4

反応物 2

HCID 31187N-CarbethoxyphthalimideHCID 28287855-Benzyloxytryptamine hydrochloride

生成物 1

HCID 1548084HCID 1548084、化合物収率 99.3%

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

実験手順

To a stirred suspension of 5-benzyloxytryptamine hydrochloride (1.0 g in 10 mL of dry tetrahydrofuran) was added triethylamine (0.50 mL) followed by N-carbethoxyphthalimide (750 mg) and the mixture heated to reflux on an oil bath. After 48 hours the reaction was cooled to room temperature, filtered and the filtrate concentrated in vacuo. The resulting solid was suspended in a mixture of hexane/methylene chloride (2.5:1, 50 mL) and filtered to give the title compound (1.3 g).

後処理

  1. temperaturethe mixture heated
  2. temperatureto reflux on an oil bath
  3. filtrationfiltered
  4. concentrationthe filtrate concentrated in vacuo
  5. additionThe resulting solid was suspended in a mixture of hexane/methylene chloride (2.5:1, 50 mL)
  6. filtrationfiltered

出典と根拠

ORDレコード
ord-bea80c8fdbdc48d694ab946c96ce418f
出典データセット
uspto-grants-2001_03
特許番号
US06197975B1

反応ノート

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