Ethyl isocyanate → HCID 86752673、化合物

HRID 1292393ノート

反応式

HRID 1292393 の反応式
[CH2:1]([O:8][C:9](=[O:49])[N:10]([CH2:31][CH2:32][CH2:33][CH2:34][C:35]1[CH:40]=[CH:39][C:38]([O:41][CH2:42][C:43]2[CH:48]=[CH:47][CH:46]=[CH:45][CH:44]=2)=[CH:37][CH:36]=1)[CH2:11][CH2:12][C:13]1[C:21]2[C:16](=[CH:17][CH:18]=[C:19]([OH:22])[CH:20]=2)[NH:15][C:14]=1[C:23]1[CH:28]=[C:27]([CH3:29])[CH:26]=[C:25]([CH3:30])[CH:24]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:50]([N:52]=[C:53]=[O:54])[CH3:51]>>[CH2:1]([O:8][C:9]([N:10]([CH2:31][CH2:32][CH2:33][CH2:34][C:35]1[CH:40]=[CH:39][C:38]([O:41][CH2:42][C:43]2[CH:44]=[CH:45][CH:46]=[CH:47][CH:48]=2)=[CH:37][CH:36]=1)[CH2:11][CH2:12][C:13]1[C:21]2[C:16](=[CH:17][CH:18]=[C:19]([O:22][C:53](=[O:54])[NH:52][CH2:50][CH3:51])[CH:20]=2)[NH:15][C:14]=1[C:23]1[CH:24]=[C:25]([CH3:30])[CH:26]=[C:27]([CH3:29])[CH:28]=1)=[O:49])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

3

反応物 2

HCID 8022Ethyl isocyanate2 回HCID 70227002HCID 70227002、化合物

生成物 1

HCID 86752673HCID 86752673、化合物

実験手順

To a solution of [4-(4-benzyloxyphenyl)-butyl]-[2-[2-(3,5-dimethylphenyl)-5-hydroxy-1H-indol-3-yl]ethyl]carbamic acid benzyl ester (50 mg in 0.5 mL dry tetrahydrofuran) was added 0.035 mL of ethyl isocyanate and the mixture stirred at room temperature. Over the course of 2 weeks, additional ethyl isocyanate was added in portions and the mixture heated to reflux for several days after which time it was cooled to room temperature, concentrated in vacuo and purified by flash chromatography on silica gel (hexane:ethyl acetate, 2:1) to give the title compound (20 mg).

後処理

  1. temperaturethe mixture heated
  2. temperatureto reflux for several days after which time it
  3. temperaturewas cooled to room temperature
  4. concentrationconcentrated in vacuo
  5. custompurified by flash chromatography on silica gel (hexane:ethyl acetate, 2:1)

出典と根拠

ORDレコード
ord-53290def764c41fcaab29989505d1493
出典データセット
uspto-grants-1998_05
特許番号
US05756507

反応ノート

読み込み中…