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Etolotifen → HCID 88677769, compound

HRID 64642
Notes
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Reaction equation

HRID 64642 reaction equation
[OH:1][CH2:2][CH2:3][O:4][CH2:5][CH2:6][O:7][CH2:8][CH2:9][N:10]1[CH2:15][CH2:14][C:13](=[C:16]2[C:25]3[CH:24]=[CH:23][S:22][C:21]=3[C:20](=O)[CH2:19][C:18]3[CH:27]=[CH:28][CH:29]=[CH:30][C:17]2=3)[CH2:12][CH2:11]1.Cl.[NH2:32][OH:33]>N1C=CC=CC=1>[OH:1][CH2:2][CH2:3][O:4][CH2:5][CH2:6][O:7][CH2:8][CH2:9][N:10]1[CH2:11][CH2:12][C:13](=[C:16]2[C:25]3[CH:24]=[CH:23][S:22][C:21]=3[C:20](=[N:32][OH:33])[CH2:19][C:18]3[CH:27]=[CH:28][CH:29]=[CH:30][C:17]2=3)[CH2:14][CH2:15]1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

4

Reactant 2

HCID 208944EtolotifenHCID 443297Hydroxyamine hydrochloride

Product 1

HCID 88677769HCID 88677769, compound

Reagents, catalysts & solvents 1

HCID 1049PyridineSolvent

Procedure

6.0 g 4-{1-[2-[2-(2-hydroxyethoxy)ethoxy]ethyl]piperidin-4-ylidene}-4H-benzo[4,5]cyclohepta[1,2-b]thiophen-10(9H)one and 0.95 g hydroxylaminehydrochlorid in 70 ml pyridine are refluxed for 12 hours. After elimination of the pyridine by distillation, ethanol and a little water are added to the residue and the title compound is crystallised out as the hydrochlorid (Mt. p. 240°-243°).

Workup

  1. distillationAfter elimination of the pyridine by distillation, ethanol
  2. additiona little water are added to the residue
  3. customthe title compound is crystallised out as the hydrochlorid (Mt. p. 240°-243°)

Sources & evidence

ORD record
ord-9b5eeadbce104826b84ebbbb115145a7
Source dataset
uspto-grants-1986_09
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US04609664

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes