Ammonia → Medazepam

HRID 441939

反応式

HRID 441939 の反応式
B#B.[CH3:3][N:4]1[C:10]2[CH:11]=[CH:12][C:13]([Cl:15])=[CH:14][C:9]=2[C:8]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)=[N:7][CH2:6][C:5]1=O.Cl.N>O1CCCC1>[CH3:3][N:4]1[C:10]2[CH:11]=[CH:12][C:13]([Cl:15])=[CH:14][C:9]=2[C:8]([C:16]2[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=2)=[N:7][CH2:6][CH2:5]1

参加物

6

反応物 4

HCID 222AmmoniaHCID 313Hydrochloric AcidHCID 3016DiazepamHCID 6328200Diboron

生成物 1

HCID 4041Medazepam収率 99.3%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
-10 °C

実験手順

To a solution of 30 ml of 1.07 M diborane in tetrahydrofuran was added with stirring 1.43 g of 1-methyl-5-phenyl-7-chloro-1,3-dihydro-2H-1,4-benzodiazepin-2-one at -15° to -10° C. After further stirring at -10° C for 2 hours, the reaction mixture was poured into 100 ml of ice-water and 20 ml of concentrated hydrochloric acid was added thereto. The mixture was reflexed for one hour. After having been cooled, the resultant red solution was neutralized with 28%-aqueous ammonia, and then extracted with ether. The ether extract was washed with water and dried over anhydrous sodium sulfate, and the solvent was removed under reduced pressure. There were obtained 1.35 g of 1-methyl-5-phenyl-7-chloro-2,3-dihydro-1H-1,4-benzodiazepine, which were recrystallized from n-hexane to give prisms melting at 99.5° to 101,0° C.

後処理

  1. additionwas added
  2. waitThe mixture was reflexed for one hour
  3. temperatureAfter having been cooled
  4. extractionextracted with ether
  5. extractionThe ether extract
  6. washwas washed with water
  7. dry with materialdried over anhydrous sodium sulfate
  8. customthe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-77475ec902224a74a78976d778490fb4
出典データセット
uspto-grants-1977_08
特許番号
US04044003

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