Hydrochloric Acid → HCID 13632831, compound

HRID 1198721Notes

Reaction equation

HRID 1198721 reaction equation
[C:1]([C:3]1[C:4]([N:15]2[CH2:20][CH2:19][O:18][CH2:17][CH2:16]2)=[N:5][CH:6]=[C:7]([C:9]2[CH:14]=[CH:13][N:12]=[CH:11][CH:10]=2)[CH:8]=1)#[N:2].[ClH:21]>O>[OH2:18].[ClH:21].[C:1]([C:3]1[C:4]([N:15]2[CH2:20][CH2:19][O:18][CH2:17][CH2:16]2)=[N:5][CH:6]=[C:7]([C:9]2[CH:10]=[CH:11][N:12]=[CH:13][CH:14]=2)[CH:8]=1)#[N:2]

Participants

4

Conditions

Temperature
50 °C

Procedure

5.0 kg 3-cyano-2-morpholino-5-(pyrid-4-yl)-pyridine is mixed with 25 l water and 2.0 l technical grade hydrochloric acid and is then heated to about 50° C. 3.01 hydrochloric acid is added to the yellow solution, which is then cooled. After crystallization, stirring is continued for a further 2 hours at temperatures below 20° C. The crystalline material is centrifuged off and washed with a mixture of 5.4 l water and 0.6 l hydrochloric acid. The yield is 5.3 kg (88% of the theoretical yield).

Workup

  1. temperatureis then cooled
  2. customAfter crystallization
  3. washwashed with a mixture of 5.4 l water and 0.6 l hydrochloric acid
  4. customThe yield is 5.3 kg (88% of the theoretical yield)

Sources & evidence

ORD record
ord-9201798980c840e096b40697b94cc4fe
Source dataset
uspto-grants-1994_01
Patent number
US05281705

Reaction notes

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