Water → HCID 54570731, 화합물

HRID 2254053노트

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HRID 2254053 반응식
O1CCOCC1.O.Cl.[CH2:9]([O:11][C:12](=[O:15])[CH2:13][NH2:14])[CH3:10].[F:16][C:17]1[C:18]([F:29])=[CH:19][C:20]2[NH:25]C(=O)[O:23][C:22](=O)[C:21]=2[CH:28]=1>C(N(CC)CC)C>[NH2:25][C:20]1[CH:19]=[C:18]([F:29])[C:17]([F:16])=[CH:28][C:21]=1[C:22]([NH:14][CH2:13][C:12]([O:11][CH2:9][CH3:10])=[O:15])=[O:23]

참가 물질

6

반응물 4

HCID 962WaterHCID 312751,4-DioxaneHCID 2723640Glycine ethyl ester, hydrochlorideHCID 109324446,7-Difluoroisatoic anhydride

생성물 1

HCID 54570731HCID 54570731, 화합물수율 71.1%

시약·촉매·용매 1

HCID 8471Triethylamine용매

반응 조건

온도
70 °C

실험 절차

Into a mixed liquor of 280 ml of dioxane with 70 ml of water were dissolved 19 g of glycine ethyl ester hydrochloride, and 21.7 g of 6,7-difluoro-2H-3,1-benzoxazine-2,4(1H)-dione were added and 14.7 g of triethylamine were added dropwise at room temperature under stirring. After stirring further for 30 minutes, the mixture was heated to 70° C. and stirred for 1,5 hours. Dioxane was distilled off, 150 ml of water were added, then the crystals deposited were collected by filtration, washed with water, and dried. They were recrystallized from ethyl acetate to obtain 20 g of title compound. m.p. 147° C.

후처리

  1. additionwere added
  2. stirringAfter stirring further for 30 minutes
  3. stirringstirred for 1,5 hours
  4. distillationDioxane was distilled off
  5. addition150 ml of water were added
  6. filtrationthe crystals deposited were collected by filtration
  7. washwashed with water
  8. customdried
  9. customThey were recrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-5aa05dd1b1294ab4855c95f2c16f9e3d
출처 데이터셋
uspto-grants-1993_08
특허 번호
US05234928

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