Potassium Iodide → HCID 21437288, 화합물

HRID 596368

반응식

HRID 596368 반응식
[OH-].[K+].Cl.[CH:4]1([CH2:7][NH2:8])[CH2:6][CH2:5]1.[F:9][C:10]([F:35])([F:34])[C:11]1[CH:12]=[CH:13][C:14]2[N:20]3[C:21]([CH2:24]Cl)=[N:22][N:23]=[C:19]3[CH2:18][N:17]=[C:16]([C:26]3[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=3[Cl:32])[C:15]=2[CH:33]=1.[I-].[K+]>CO.O1CCCC1>[F:35][C:10]([F:9])([F:34])[C:11]1[CH:12]=[CH:13][C:14]2[N:20]3[C:21]([CH2:24][NH:8][CH2:7][CH:4]4[CH2:6][CH2:5]4)=[N:22][N:23]=[C:19]3[CH2:18][N:17]=[C:16]([C:26]3[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=3[Cl:32])[C:15]=2[CH:33]=1

참가 물질

7

반응물 4

HCID 4875Potassium IodideHCID 14797Potassium HydroxideHCID 81671(Cyclopropylmethyl)ammonium chlorideHCID 213307808-(trifluoromethyl)-1-(chloromethyl)-6-(o-chlorophenyl)-4H-s-triazolo[4,3-a][1,4]benzodiazepine

생성물 1

HCID 21437288HCID 21437288, 화합물

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

실험 절차

A stirred solution of potassium hydroxide (3.37 g., 0.06 mole) in methanol (30 ml.) is cooled in an ice bath, under nitrogen, and treated with (cyclopropylmethyl)-amine hydrochloride (6.45 g., 0.06 mole). The resulting mixture is kept in the ice bath for 15 minutes, treated with tetrahydrofuran (250 ml.), 8-(trifluoromethyl)-1-(chloromethyl)-6-(o-chlorophenyl)-4H-s-triazolo[4,3-a][1,4]benzodiazepine (6.86 g., 0.02 mole) and potassium iodide (3.32 g., 0.02 mole) and kept at ambient temperature for 18 hours. The mixture is concentrated and the residue is mixed with water and extracted with methylene chloride. The extract is washed with brine, dried over anhydrous sodium sulfate and concentrated. The product is crystallized once from ethyl acetate and once from methylene chloride ethyl acetate to give 8-(trifluoromethyl)-1-[[(cyclopropylmethyl)amino]methyl]-6-(o-chlorophenyl)-4H-s-triazolo[4,3-a][1,4]benzodiazepine. Preparation 28 8 -Chloro-1-[[(cyclopropylmethyl)amino] methyl]-6-(o-chlorophenyl)-4H-s-triazolo[4,3-a][1,4]benzodiazepine

후처리

  1. concentrationThe mixture is concentrated
  2. additionthe residue is mixed with water
  3. extractionextracted with methylene chloride
  4. washThe extract is washed with brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated
  7. customThe product is crystallized once from ethyl acetate and once from methylene chloride ethyl acetate

출처 및 근거

ORD 기록
ord-b85af1f64e684f52a0aff5d18ad57932
출처 데이터셋
uspto-grants-1977_03
특허 번호
US04010177

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