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Hydrochloric Acid → HCID 20542099, 화합물

HRID 2286163
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HRID 2286163 반응식
C[Li].[F:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[C:10]1[C:16]2[CH:17]=[C:18]([C:21]#N)[CH:19]=[CH:20][C:15]=2[NH:14][C:13](=[O:23])[CH:12]([CH3:24])[N:11]=1.Cl.[OH-:26].[Na+].[CH3:28]COCC>O1CCCC1>[C:21]([C:18]1[CH:19]=[CH:20][C:15]2[NH:14][C:13](=[O:23])[CH:12]([CH3:24])[N:11]=[C:10]([C:5]3[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=3[F:3])[C:16]=2[CH:17]=1)(=[O:26])[CH3:28]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 14798Sodium HydroxideHCID 20542076HCID 20542076, 화합물HCID 178418348HCID 178418348, 화합물

생성물 1

HCID 20542099HCID 20542099, 화합물

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매

실험 절차

110 ml of a 2 N solution of methyl lithium in ether are added dropwise to a solution, stirred at -70° under argon, of 12.81 g (43.68 mmol) of 5-(o-fluorophenyl)-2,3-dihydro-3-methyl-2-oxo-1H-1,4-benzodiazepine-7-carbonitrile in 500 ml of tetrahydrofuran. After 21 hours at -70°, 440 ml of 2 N hydrochloric acid are added thereto at -70° and, after warming to room temperature, the mixture is neutralised with 135 ml of 3 N sodium hydroxide. After separating the aqueous phase, the organic phase is evaporated at 40° in vacuo, the residue is taken up in methylene chloride and the organic phase is washed with the aqueous phase separated above. The methylene chloride solution is washed with water, dried and evaporated. The residue yields, from methylene chloride/cyclohexane, 7-acetyl-5-(o-fluorophenyl)-1,3-dihydro-3-methyl-2H-1,4-benzodiazepin-2-one of melting point 203°.

후처리

  1. customAfter separating the aqueous phase
  2. customthe organic phase is evaporated at 40° in vacuo
  3. washthe organic phase is washed with the aqueous phase
  4. customseparated above
  5. washThe methylene chloride solution is washed with water
  6. customdried
  7. customevaporated

출처 및 근거

ORD 기록
ord-75add84b15944f81bbc9bf0b5d0ffc41
출처 데이터셋
uspto-grants-1982_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04327026

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