Ammonium Hydroxide → HCID 22748787, compound

HRID 1390331Notes

Reaction equation

HRID 1390331 reaction equation
[C:1]1([CH:7]([C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)[C:8]2[C:9](=O)[NH:10][CH:11]=[C:12]([CH:14]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)[C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)[CH:13]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C1(P(Cl)([Cl:42])=O)C=CC=CC=1.[OH-].[NH4+]>>[Cl:42][C:9]1[C:8]([CH:7]([C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)[C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)=[CH:13][C:12]([CH:14]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[C:15]2[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=2)=[CH:11][N:10]=1

Participants

4

Reactant 3

HCID 14923Ammonium HydroxideHCID 69990Phenylphosphonic dichlorideHCID 22748752HCID 22748752, compound

Product 1

HCID 22748787HCID 22748787, compound

Procedure

Combine 49.5 g. (0.11 moles) of 3,5-bis-(diphenylmethyl)-2-pyridone (prepared as described in step B) with 105 ml. of phenylphosphonic dichloride and heat the reaction mixture with stirring at 200°-210° C. for 6 hours. Pour the reaction mixture onto ice and basify with ammonium hydroxide. Extract with ethyl ether, dry the extract and evaporate to yield a residue which is crystallized from ethanol to yield the product of this step, yield about 40 g., m.p. 131°-133° C.

Workup

  1. additionPour the reaction mixture onto ice
  2. extractionExtract with ethyl ether
  3. customdry the
  4. extractionextract
  5. customevaporate
  6. customto yield a residue which
  7. customis crystallized from ethanol
  8. customto yield the product of this step, yield about 40 g

Sources & evidence

ORD record
ord-557304fb404147e98d96b774ef324fb0
Source dataset
uspto-grants-1979_02
Patent number
US04138488

Reaction notes

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