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Triethylamine → Xaliproden Hydrochloride

HRID 1953800
ノート
印刷プレビュー

反応式

HRID 1953800 の反応式
[F:1][C:2]([F:16])([F:15])[C:3]1[CH:4]=[C:5]([C:9]2[CH2:10][CH2:11][NH:12][CH2:13][CH:14]=2)[CH:6]=[CH:7][CH:8]=1.C(N(CC)CC)C.Br[CH2:25][CH2:26][C:27]1[CH:36]=[CH:35][C:34]2[C:29](=[CH:30][CH:31]=[CH:32][CH:33]=2)[CH:28]=1.[Cl:37]CCC1C=CC2C(=CC=CC=2)C=1>C(O)C>[ClH:37].[CH:28]1[C:29]2[C:34](=[CH:33][CH:32]=[CH:31][CH:30]=2)[CH:35]=[CH:36][C:27]=1[CH2:26][CH2:25][N:12]1[CH2:11][CH:10]=[C:9]([C:5]2[CH:6]=[CH:7][CH:8]=[C:3]([C:2]([F:1])([F:15])[F:16])[CH:4]=2)[CH2:14][CH2:13]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 8471TriethylamineHCID 2282702-(2-Bromoethyl)naphthaleneHCID 111280344-[3-(Trifluoromethyl)phenyl]-1,2,3,6-tetrahydropyridineHCID 12698954HCID 12698954、化合物

生成物 1

HCID 128918Xaliproden Hydrochloride収率 59.8%

試薬・触媒・溶媒 1

HCID 702
Ethanol
溶媒

実験手順

In two different preparations, 4-(3-trifluoromethylphenyl)-1,2,3,6-tetrahydropyridine is reacted, in the presence of triethylamine, with 2-(2-bromoethyl)naphthalene (PREPARATION A) and respectively with 2-(2-chloroethyl)naphthalene (PREPARATION B) in ethanol under reflux for 20 hours. The reaction mixtures of the two preparations were concentrated, the residue was taken up with ethyl ether and the ether solution, which was filtered and washed with water, was dried and evaporated. The residue was taken up with a solution of gaseous hydrochloric acid in isopropanol to give 1-[2-(2-naphthyl)ethyl]-4-(3-trifluoromethylphenyl)-1,2,3,6-tetrahydropyridine hydrochloride, which was crystallized from ethanol.

後処理

  1. temperatureunder reflux for 20 hours
  2. customThe reaction mixtures of the two preparations
  3. concentrationwere concentrated
  4. filtrationthe ether solution, which was filtered
  5. washwashed with water
  6. customwas dried
  7. customevaporated

出典と根拠

ORDレコード
ord-7891de4724cf45bbad362ebdd627910b
出典データセット
uspto-grants-2000_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06118006

反応ノート

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