Water → HCID 54570731、化合物

HRID 2254053ノート

反応式

HRID 2254053 の反応式
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]

参加物

6

反応物 4

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

生成物 1

HCID 54570731HCID 54570731、化合物収率 71.1%

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

反応条件

温度
70 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5aa05dd1b1294ab4855c95f2c16f9e3d
出典データセット
uspto-grants-1993_08
特許番号
US05234928

反応ノート

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