Triethylamine → HCID 20500933, compound

HRID 851758Notes

Reaction equation

HRID 851758 reaction equation
Cl.[OH:2][CH2:3][CH2:4][CH:5]1[CH2:14][C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[C:7]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)=[N:6]1.[CH2:21](N(CC)CC)C.S(Cl)(C)(=O)=O>C(Cl)Cl>[OH:2][CH2:3][CH2:4][CH:5]1[CH2:14][C:13]2[C:8](=[CH:9][C:10]([CH3:21])=[CH:11][CH:12]=2)[C:7]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)=[N:6]1

Participants

5

Reactant 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 20500932HCID 20500932, compound

Product 1

HCID 20500933HCID 20500933, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

To a solution cooled to -10° C. of 9 g of the compound of formula (XXXI) obtained in the preceding step and 12.5 ml of triethylamine in 250 ml of methylene chloride are added 5.4 ml of mesyl chloride. Then it is left for 30 minutes at ambient temperature, then washed with water with the help of 1 N hydrochloric acid solution, with water, with a sodium bicarbonate solution, dried on sodium sulfate, filtered and the filtrate is evaporated. An oil is obtained which is then crystallized.

Workup

  1. washwashed with water with the help of 1 N hydrochloric acid solution, with water, with a sodium bicarbonate solution
  2. customdried on sodium sulfate
  3. filtrationfiltered
  4. customthe filtrate is evaporated
  5. customAn oil is obtained which
  6. customis then crystallized

Sources & evidence

ORD record
ord-ec7aa729f2af4b1bbf86009b40026936
Source dataset
uspto-grants-1983_05
Patent number
US04386090

Reaction notes

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