1,4-Dioxane hydrochloride → HCID 68421313, compound

HRID 2061215Notes

Reaction equation

HRID 2061215 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

Reactant 2

HCID 204431481,4-Dioxane hydrochlorideHCID 59853868HCID 59853868, compound

Product 1

HCID 68421313HCID 68421313, compound

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-7a40e2fdae5c42fb9ec86cb690989a41
Source dataset
uspto-grants-2012_10
Patent number
US08278329B2

Reaction notes

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