Ethylene Glycol → HCID 21416142, compound

HRID 1075868Notes

Reaction equation

HRID 1075868 reaction equation
C([N:6]1[CH2:11][CH2:10][N:9]([CH:12]2[C:18]3[CH:19]=[C:20]([F:23])[CH:21]=[CH:22][C:17]=3[S:16][C:15]3[CH:24]=[CH:25][C:26]([Cl:28])=[CH:27][C:14]=3[CH2:13]2)[CH2:8][CH2:7]1)(OCC)=O.C(O)CO.[OH-].[K+]>O>[Cl:28][C:26]1[CH:25]=[CH:24][C:15]2[S:16][C:17]3[CH:22]=[CH:21][C:20]([F:23])=[CH:19][C:18]=3[CH:12]([N:9]3[CH2:10][CH2:11][NH:6][CH2:7][CH2:8]3)[CH2:13][C:14]=2[CH:27]=1

Participants

5

Reactant 3

HCID 174Ethylene GlycolHCID 14797Potassium HydroxideHCID 21416190HCID 21416190, compound

Product 1

HCID 21416142HCID 21416142, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent2×

Procedure

24.5 G. of 1-carbethoxy-4-(2-chloro-8-fluoro-10,11-dihydro-dibenzo[b,f]thiepin-10-yl)-piperazine, 350 ml. of ethyleneglycol, 19 g. of potassium hydroxide and 1.5 ml. of water are heated together at 160° for 1 hours. The reaction mixture is poured over water and extracted with chloroform. The organic phase is washed with water, dried over magnesium sulfate and evaporated under reduced pressure, whereby there is obtained 1-(2-chloro-8-fluoro-10,11-dihydro-dibenzo-[b,f]thiepin-10-yl)-piperazine as a thick oil.

Workup

  1. extractionextracted with chloroform
  2. washThe organic phase is washed with water
  3. dry with materialdried over magnesium sulfate
  4. customevaporated under reduced pressure

Sources & evidence

ORD record
ord-249d2c39e8324131b33b0c789f0d1281
Source dataset
uspto-grants-1976_05
Patent number
US03954764

Reaction notes

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