Dimethyl Sulfate → HCID 20364766、化合物

HRID 1973296ノート

反応式

HRID 1973296 の反応式
[F:1][C:2]([F:22])([F:21])[C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([C:9]2[C:15]3[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=3[NH:13][C:12](=[O:20])[CH2:11][N:10]=2)[CH:4]=1.[CH3:23]OS(OC)(=O)=O>CC(C)=O>[CH3:23][N:13]1[C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=2[C:9]([C:5]2[CH:4]=[C:3]([C:2]([F:1])([F:21])[F:22])[CH:8]=[CH:7][CH:6]=2)=[N:10][CH2:11][C:12]1=[O:20]

参加物

4

反応物 2

HCID 6497Dimethyl SulfateHCID 23275906HCID 23275906、化合物

生成物 1

HCID 20364766HCID 20364766、化合物

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A solution of 15.2 g. of 1,3-dihydro-5-(α,α,α-trifluoro-m-tolyl)-2H-1,4-benzodiazepin-2-one in 360ml. of acetone is treated with 7.5 ml. of dimethylsulfate and 45 g. of finely triturated, dry potassium carbonate and stirred intensively at room temperature for 15 hours. The mixture is then poured into 400 ml. of ice-water, the acetone is evaporated under reduced pressure and the separated oil extracted with methylene chloride. The extract is washed with water, dried over sodium sulfate and evaporated to dryness. The resulting oil crystallizes on trituration with hexane, and there is obtained 1,3-dihydro-1-methyl-5-(α,α,α-trifluoro-m-tolyl)-2H-1,4-benzodiazepin-2-one having a melting point of 117°-119° C., which can be employed in the next stage without further purification. A sample for analysis is obtained by crystallization from ethanol; melting point 121°-122° C.

後処理

  1. customof finely triturated
  2. additionThe mixture is then poured into 400 ml
  3. customof ice-water, the acetone is evaporated under reduced pressure
  4. extractionthe separated oil extracted with methylene chloride
  5. washThe extract is washed with water
  6. dry with materialdried over sodium sulfate
  7. customevaporated to dryness
  8. customThe resulting oil crystallizes on trituration with hexane

出典と根拠

ORDレコード
ord-55f63a5b018841489191afe06533bfcc
出典データセット
uspto-grants-1976_12
特許番号
US03996374

反応ノート

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