Anisole → HCID 12703444, compound

HRID 1855732Notes

Reaction equation

HRID 1855732 reaction equation
[CH3:1][N:2]1[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.C1(OC)C=CC=CC=1.[F:16][C:17]1[CH:18]=[CH:19][C:20]2[NH:26][C:25]3=[CH:27][S:28][CH:29]=[C:24]3[NH:23][C:22](=O)[C:21]=2[CH:31]=1>[Ti](Cl)(Cl)(Cl)Cl.C1(C)C=CC=CC=1>[F:16][C:17]1[CH:18]=[CH:19][C:20]2[NH:26][C:25]3=[CH:27][S:28][CH:29]=[C:24]3[N:23]=[C:22]([N:5]3[CH2:6][CH2:7][N:2]([CH3:1])[CH2:3][CH2:4]3)[C:21]=2[CH:31]=1

Participants

6

Reactant 3

HCID 7519AnisoleHCID 531671-Methylpiperazine2×HCID 12680131HCID 12680131, compound

Product 1

HCID 12703444HCID 12703444, compound

Reagents, catalysts & solvents 2

HCID 24193Titanium TetrachlorideCatalystHCID 1140TolueneSolvent2×

Procedure

To a stirred mixture of 14.0 g. of N-methylpiperazine, 3.4 ml. of titanium tetrachloride and 6 ml. of anisole in 60 ml. of toluene is added a mixture of 6.7 g. of N-methylpiperazine and 5.6 g. of 7-fluoro-4H-thieno[3,4-b][1,4]benzodiazepin-9(10H)-one in 6 ml. of toluene. The mixture is treated as described in Example 1, giving the desired product as a tan solid, m.p. 224°-227° C. (dec.).

Workup

  1. additionTo a stirred mixture of 14.0 g
  2. additiona mixture of 6.7 g
  3. additionThe mixture is treated

Sources & evidence

ORD record
ord-2187d5f9ae88468ab694593a3f6cf1f4
Source dataset
uspto-grants-1980_08
Patent number
US04216148

Reaction notes

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