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Hydrochloric Acid → 10-[2-(Diethylamino)ethyl]-5-ethyl-10,11-dihydro-5H-dibenzo[b,f]azepine-10-carbonitrile--hydrogen chloride (1/1)

HRID 1287597
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HRID 1287597 반응식
[CH2:1]([N:3]([CH2:25][CH3:26])[CH2:4][CH2:5][C:6]1([C:23]#[N:24])[C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=2[N:10]([CH2:17][CH3:18])[C:9]2[CH:19]=[CH:20][CH:21]=[CH:22][C:8]=2[CH2:7]1)[CH3:2].[ClH:27]>CC(O)C>[ClH:27].[CH2:25]([N:3]([CH2:1][CH3:2])[CH2:4][CH2:5][C:6]1([C:23]#[N:24])[C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=2[N:10]([CH2:17][CH3:18])[C:9]2[CH:19]=[CH:20][CH:21]=[CH:22][C:8]=2[CH2:7]1)[CH3:26]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 431312HCID 431312, 화합물

생성물 1

HCID 1231858310-[2-(Diethylamino)ethyl]-5-ethyl-10,11-dihydro-5H-dibenzo[b,f]azepine-10-carbonitrile--hydrogen chloride (1/1)

시약·촉매·용매 1

HCID 3776Isopropanol용매2회

실험 절차

A solution of 10 parts of 10-[2-(diethylamino)ethyl]-5-ethyl-10,11-dihydro-5H-dibenz[b,f]azepine-10-carbonitrile in a minimal amount of 2-propanol is acidified with approximately 20% hydrogen chloride dissolved in 2-propanol. Precipitation occurs. Sufficient anhydrous ether is introduced to ensure completion of the precipitation, whereupon the insoluble solids are filtered off, washed with anhydrous ether, dried in air, and recrystallized from absolute ethanol to give 10-[2-(diethylamino)ethyl]-5-ethyl-10,11-dihydro-5H-dibenz[b,f]azepine-10-carbonitrile hydrochloride as a colorless solid melting at 211°-214°.

후처리

  1. customPrecipitation
  2. additionSufficient anhydrous ether is introduced
  3. customcompletion of the precipitation
  4. filtrationwhereupon the insoluble solids are filtered off
  5. washwashed with anhydrous ether
  6. customdried in air
  7. customrecrystallized from absolute ethanol

출처 및 근거

ORD 기록
ord-9a919ac77ff0481eaddc69352670ca13
출처 데이터셋
uspto-grants-1976_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03985730

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