Ethyl isocyanate → HCID 54539808, 화합물

HRID 894465노트

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HRID 894465 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 54539808HCID 54539808, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-12c8355f12324f1eaf822af12244354c
출처 데이터셋
uspto-grants-1981_08
특허 번호
US04284555

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