Tetrahydrofuran → HCID 14098866, compound

HRID 1165131Notes

Reaction equation

HRID 1165131 reaction equation
[CH:1]([O:14][CH2:15][CH2:16][N:17]1[CH2:22][CH2:21][N:20]([CH2:23][CH2:24][N:25]2[C:29](=[O:30])[C:28]3=[CH:31][CH:32]=[CH:33][CH:34]=[C:27]3[C:26]2=[O:35])[CH2:19][CH2:18]1)([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[O:36]1CCCC1>O>[CH:1]([O:14][CH2:15][CH2:16][N:17]1[CH2:22][CH2:21][N:20]([CH2:23][CH2:24][NH:25][C:26](=[O:35])[C:27]2[CH:34]=[CH:33][CH:32]=[CH:31][C:28]=2[C:29]([OH:36])=[O:30])[CH2:19][CH2:18]1)([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Participants

4

Reactant 2

HCID 8028TetrahydrofuranHCID 3087861HCID 3087861, compound

Product 1

HCID 14098866HCID 14098866, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

20 g of 1-[2-(benzhydryloxy)ethyl]-4-[2-(phthalimido)ethyl]piperazine and 200 ml of tetrahydrofuran were placed in a reactor. A solution of 20.4 g of Na2S.9H2O in 80 ml of water was added dropwise at 0° C. After decantation, the solvents were evaporated off. The solid was taken up in 50 ml of water and 100 ml of methylene chloride. After the solution had cooled, the pH was adjusted to 3.7 and extraction was carried out with 2 times 50 ml of methylene chloride. After drying, the solvents were evaporated off to give 17 g of a solid (m.p.=45° C.) of the empirical formula: C29H33N3O4.

Workup

  1. customAfter decantation, the solvents were evaporated off
  2. temperatureAfter the solution had cooled
  3. extractionthe pH was adjusted to 3.7 and extraction
  4. customAfter drying
  5. customthe solvents were evaporated off

Sources & evidence

ORD record
ord-cd03f7256b0a46bcadf5e67071b26341
Source dataset
uspto-grants-1990_03
Patent number
US04908365

Reaction notes

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