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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
ノート
印刷プレビュー

反応式

HRID 1287597 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 431312HCID 431312、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒2 回

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-9a919ac77ff0481eaddc69352670ca13
出典データセット
uspto-grants-1976_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03985730

反応ノート

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