Ethyl isocyanate → HCID 54539808、化合物

HRID 894465ノート

反応式

HRID 894465 の反応式
[Cl:1][C:2]1[C:19]([OH:20])=[CH:18][C:5]2[C@H:6]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[CH2:7][N:8]([CH3:11])[CH2:9][CH2:10][C:4]=2[CH:3]=1.[CH2:21]([N:23]=[C:24]=[O:25])[CH3:22]>C(#N)C>[Cl:1][C:2]1[C:19]([O:20][C:24]([NH:23][CH2:21][CH3:22])=[O:25])=[CH:18][C:5]2[C@H:6]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[CH2:7][N:8]([CH3:11])[CH2:9][CH2:10][C:4]=2[CH:3]=1

参加物

4

反応物 2

HCID 8022Ethyl isocyanateHCID 6603800(5S)-8-Chloro-2,3,4,5-tetrahydro-3-methyl-5-phenyl-1H-3-benzazepin-7-ol

生成物 1

HCID 54539808HCID 54539808、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

Dissolve 1.22 g (0.0042 moles) of the product of step E in 60 ml of refluxing acetonitrile and add dropwise 0.6 ml of ethyl isocyanate with stirring. Reflux for 30 minutes after addition is complete. Evaporate to dryness and crystallize the residue from acetonitrile to obtain analytically pure (S)-7-chloro-8-(ethylaminocarbonyloxy)-3-methyl-1-phenyl-2,3,4,5-tetrahydro-1H-3-benzazepine, m.p. 133°-134.5° C. [α]D26 =+20.2° (c=0.5, ethanol).

後処理

  1. temperatureReflux for 30 minutes
  2. additionafter addition
  3. customEvaporate to dryness
  4. customcrystallize the residue from acetonitrile

出典と根拠

ORDレコード
ord-12c8355f12324f1eaf822af12244354c
出典データセット
uspto-grants-1981_08
特許番号
US04284555

反応ノート

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