Hydrochloric Acid → HCID 178527725, 화합물

HRID 540344노트

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HRID 540344 반응식
Cl[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[N:5]=[C:4]([N:12]2[CH2:18][CH2:17][CH2:16][C:15]3[CH:19]=[CH:20][CH:21]=[CH:22][C:14]=3[CH2:13]2)[CH:3]=1.C[S-:24].[Na+].Cl>CN(C)C=O.O>[CH2:13]1[C:14]2[CH:22]=[CH:21][CH:20]=[CH:19][C:15]=2[CH2:16][CH2:17][CH2:18][N:12]1[C:4]1[CH:3]=[C:2]([SH:24])[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[N:5]=1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 4378561Sodium methanethiolateHCID 71255109HCID 71255109, 화합물

생성물 1

HCID 178527725HCID 178527725, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

반응 조건

온도
50 °C

실험 절차

A mixture of 2-(4-chloroquinolin-2-yl)-2,3,4,5-tetrahydro-1H-2-benzazepine (2 g, 6.47 mmol) and sodium thiomethoxide (2.4 g, 34 mmol) in dry N,N-dimethylformamide (20 mL) was heated with stirring overnight under reflux. The reaction mixture was cooled to 50° C. and the volatile components were evaporated under reduced pressure to give a residue which was dissolved in 30 mL of chilled water and carefully acidified with 20% hydrochloride aid to pH 4-5 under argon. The resultant solution was extracted with chilled dichloromethane (30 mL×3). The dichloromethane fractions were combined and washed with chilled brine (30 mL×2) and then concentrated under reduced pressure at room temperature to give the crude product. It was used in next step without further purification.

후처리

  1. temperaturewas heated
  2. temperatureunder reflux
  3. customthe volatile components were evaporated under reduced pressure
  4. customto give a residue which
  5. extractionThe resultant solution was extracted with chilled dichloromethane (30 mL×3)
  6. washwashed with chilled brine (30 mL×2)
  7. concentrationconcentrated under reduced pressure at room temperature

출처 및 근거

ORD 기록
ord-13e6c18dc96842c194b7f82a0d51ec62
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08871756B2

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