Water → 7-chloro-3-dipropylacetoxy-5-(2'-fluorophenyl)-1,3-dihydro-2H-1,4-benzodiazepine-2-one

HRID 443794ノート

反応式

HRID 443794 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:11][C:10](=[O:12])[CH2:9][N+:8]([O-])=[C:7]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=3[F:20])[C:6]=2[CH:21]=1.[CH2:22]([CH:25]([CH2:38][CH2:39][CH3:40])[C:26]([O:28]C(=O)C(CCC)CCC)=[O:27])[CH2:23][CH3:24].C1CCCCC1.CC(C)=O.O>C(Cl)(Cl)Cl>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:11][C:10](=[O:12])[CH:9]([O:28][C:26](=[O:27])[CH:25]([CH2:38][CH2:39][CH3:40])[CH2:22][CH2:23][CH3:24])[N:8]=[C:7]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=3[F:20])[C:6]=2[CH:21]=1

参加物

6

反応物 4

HCID 962WaterHCID 109236242-Propylpentanoyl 2-propylpentanoateHCID 21916603Acetone cyclohexaneHCID 178516821HCID 178516821、化合物

生成物 1

HCID 234655657-chloro-3-dipropylacetoxy-5-(2'-fluorophenyl)-1,3-dihydro-2H-1,4-benzodiazepine-2-one

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

A suspension of 10 g of 7-chloro-5-(2'-fluoro-phenyl)-1,3-dihydro-2H-1,4-benzodiazepine-2-one-4-oxide in 20 ml of absolute chloroform is mixed with 14.3 g of dipropyl acetic acid anhydride and is heated under reflux and with the exclusion of atmospheric moisture for such a length of time until a sample on the thin layer-chromatogram (silica gel 60 F 254 of the firm Merck, flow agent: cyclohexane/acetone=1:1) shows a complete conversion. Then, the cooled mixture is shaken out several times with water, the organic phase is dried with Na2SO4 and the filtrate is evaporated in the vacuum. Upon standing over night, the residue crystallizes, is washed with petroleum ether and recrystallized from aceontrile. One will obtain a colorless powder of 7-chloro-3-dipropylacetoxy-5-(2'-fluorophenyl)-1,3-dihydro-2H-1,4-benzodiazepine-2-one, which melts at 147°-149°.

後処理

  1. temperatureis heated
  2. temperatureunder reflux and with the exclusion of atmospheric moisture for such a length of time until a sample on the thin layer-chromatogram (silica gel 60 F 254 of the firm Merck, flow agent
  3. dry with materialthe organic phase is dried with Na2SO4
  4. customthe filtrate is evaporated in the vacuum
  5. waitUpon standing over night
  6. customthe residue crystallizes
  7. washis washed with petroleum ether
  8. customrecrystallized from aceontrile

出典と根拠

ORDレコード
ord-7a5b95c8da074024975d6528edeb2885
出典データセット
uspto-grants-1981_04
特許番号
US04261987

反応ノート

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