1,4-Dioxane hydrochloride → HCID 68421313, compound

HRID 2374812Notes

Reaction equation

HRID 2374812 reaction equation
[ClH:1].O1CCOCC1.[CH:8]1[C:18]2[CH:17]=[CH:16][C:15]3[CH:19]=[CH:20][CH:21]=[CH:22][C:14]=3[C:13](=[C:23]3[CH2:28][CH2:27][N:26]([C:29](=[O:45])[CH2:30][CH2:31][N:32]([CH2:40][C:41]([CH3:44])([CH3:43])[CH3:42])C(=O)OC(C)(C)C)[CH2:25][CH2:24]3)[C:12]=2[CH:11]=[CH:10][CH:9]=1>>[ClH:1].[CH:19]1[C:15]2[CH:16]=[CH:17][C:18]3[CH:8]=[CH:9][CH:10]=[CH:11][C:12]=3[C:13](=[C:23]3[CH2:24][CH2:25][N:26]([C:29](=[O:45])[CH2:30][CH2:31][NH:32][CH2:40][C:41]([CH3:43])([CH3:42])[CH3:44])[CH2:27][CH2:28]3)[C:14]=2[CH:22]=[CH:21][CH:20]=1

Participants

3

Procedure

5 ml of 4 N hydrochloric acid/1,4-dioxane solution was added to 184.1 mg (0.357 mmol) of t-butyl 3-[4-(5H-dibenzo[a,d][7]annulen-5-ylidene)-1-piperidinyl]-3-oxopropyl(neopentyl)carbamate, and they were stirred for 1 hour. The solvent was evaporated under reduced pressure. 5 ml of diethyl ether was added to the residue, and then 1 ml of 4 N hydrochloric acid/ethyl acetate solution was added thereto. The precipitates thus formed were taken by the filtration, washed with diethyl ether and dried under reduced pressure to obtain the title compound.

Workup

  1. customThe solvent was evaporated under reduced pressure
  2. addition5 ml of diethyl ether was added to the residue
  3. addition1 ml of 4 N hydrochloric acid/ethyl acetate solution was added
  4. customThe precipitates thus
  5. customformed
  6. filtrationwere taken by the filtration
  7. washwashed with diethyl ether
  8. customdried under reduced pressure

Sources & evidence

ORD record
ord-c0de98e1cdb942f69f984c3fbc764e16
Source dataset
uspto-grants-2008_12
Patent number
US07462630B2

Reaction notes

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