Dimethylamine → 2-[2-(Dimethylamino)ethyl]-2,3-dihydro-4-methylpyrido[3,4-f][1,4]oxazepin-5(4H)-one oxalate hydrate

HRID 247312노트

반응식

HRID 247312 반응식
Cl[CH2:2][CH2:3][CH:4]1[CH2:10][N:9]([CH3:11])[C:8](=[O:12])[C:7]2[CH:13]=[N:14][CH:15]=[CH:16][C:6]=2[O:5]1.[C:17]([OH:22])(=[O:21])[C:18]([OH:20])=[O:19].[CH3:23][NH:24][CH3:25]>C(O)(C)C.O>[OH2:5].[C:17]([OH:22])(=[O:21])[C:18]([OH:20])=[O:19].[CH3:23][N:24]([CH3:25])[CH2:2][CH2:3][CH:4]1[CH2:10][N:9]([CH3:11])[C:8](=[O:12])[C:7]2[CH:13]=[N:14][CH:15]=[CH:16][C:6]=2[O:5]1

참가 물질

6

반응물 3

HCID 674Dimethylamine2회HCID 971Oxalic AcidHCID 137264002-(2-chloroethyl)-2,3-dihydro-4-methylpyrido[3,4-f][1,4]oxazepin-5(4H)-one

생성물 1

HCID 137264052-[2-(Dimethylamino)ethyl]-2,3-dihydro-4-methylpyrido[3,4-f][1,4]oxazepin-5(4H)-one oxalate hydrate

시약·촉매·용매 2

HCID 962Water용매HCID 3776Isopropanol용매

실험 절차

A solution of 5 g (0.02 mole) of 2-(2-chloroethyl)-2,3-dihydro-4-methylpyrido[3,4-f][1,4]oxazepin-5(4H)-one, in 25 ml of dimethylamine was placed in a sealed vessel and stirred for 72 hr. The vessel was opened and the excess dimethylamine allowed to evaporate. The residue was dissolved in chloroform and the solvent was stripped off in vacuo to remove excess dimethylamine. The residue was partitioned between dilute sodium hydroxide and ethyl acetate. The ethyl acetate solution was concentrated and the residue was treated with 3 g (0.033 mole) of oxalic acid in 50 ml of isopropyl alcohol and enough water to dissolve the salt while boiling. The resulting crystals were recrystallized from the same solvent. Yield of product was 5.3 g (60%), m.p. 179°-181° C.

후처리

  1. customto evaporate
  2. dissolutionThe residue was dissolved in chloroform
  3. customto remove excess dimethylamine
  4. customThe residue was partitioned between dilute sodium hydroxide and ethyl acetate
  5. concentrationThe ethyl acetate solution was concentrated
  6. dissolutionto dissolve the salt
  7. customThe resulting crystals were recrystallized from the same solvent

출처 및 근거

ORD 기록
ord-e6814a9f3e7c43b291f9a12337f83152
출처 데이터셋
uspto-grants-1987_11
특허 번호
US04705853

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