Water → 9-Chloro-7-[2-(2,4-di-t-amylphenoxy)butanoylamino]-6-hydroxy-1,5-benzodiazepin-2,4-dione

HRID 1253011

反応式

HRID 1253011 の反応式
[NH2:1][C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([N+:9]([O-])=O)=[CH:4][C:3]=1[OH:12].[C:13]([C:18]1[CH:30]=[C:29]([C:31]([CH2:34][CH3:35])([CH3:33])[CH3:32])[CH:28]=[CH:27][C:19]=1[O:20][CH:21]([CH2:25][CH3:26])[C:22](Cl)=[O:23])([CH2:16][CH3:17])([CH3:15])[CH3:14].[Cl-].[NH4+:37].[OH2:38]>C(#N)C.C(O)(C)C>[Cl:8][C:6]1[C:5]2=[N:9][C:3](=[O:12])[CH2:2][C:7](=[O:38])[N:37]=[C:4]2[C:3]([OH:12])=[C:2]([NH:1][C:22](=[O:23])[CH:21]([O:20][C:19]2[CH:27]=[CH:28][C:29]([C:31]([CH2:34][CH3:35])([CH3:33])[CH3:32])=[CH:30][C:18]=2[C:13]([CH2:16][CH3:17])([CH3:15])[CH3:14])[CH2:25][CH3:26])[CH:7]=1

参加物

7

反応物 4

HCID 962WaterHCID 25517Ammonium ChlorideHCID 1703932-(2,4-Bis(1,1-dimethylpropyl)phenoxy)butyryl chlorideHCID 38948482-Amino-4-chloro-5-nitrophenol

生成物 1

HCID 1355831249-Chloro-7-[2-(2,4-di-t-amylphenoxy)butanoylamino]-6-hydroxy-1,5-benzodiazepin-2,4-dione

試薬・触媒・溶媒 2

HCID 3776Isopropanol溶媒HCID 6342Acetonitrile溶媒

実験手順

20 g of 2-amino-4-chloro-5-nitrophenol was dispersed in 150 ml of acetonitrile, and 37.7 g of 2-(2,4-di-t-amylphenoxy)butanoyl chloride was added thereto dropwise under refluxing. After stirring while refluxing for 1 hour, the reaction mixture was cooled to room temperature, and the crystals thus formed were collected by filtration, washed with acetonitrile, and dried to obtain crystals weighing 49.5 g. A mixture of 49 g of the resulting crystals, 28 g of reduced iron, 2.7 g of ammonium chloride, 50 ml of water, and 500 ml of isopropanol was stirred while refluxing for 1 hour. The iron powder was removed by filtration, and the filtrate was cooled to precipitate crystals, which were then collected by filtration and dried to provide 42.4 g of the desired compound.

後処理

  1. temperaturedropwise under refluxing
  2. temperaturewhile refluxing for 1 hour
  3. customthe crystals thus formed
  4. filtrationwere collected by filtration
  5. washwashed with acetonitrile
  6. customdried
  7. customto obtain crystals
  8. stirringwas stirred
  9. temperaturewhile refluxing for 1 hour
  10. customThe iron powder was removed by filtration
  11. temperaturethe filtrate was cooled
  12. customto precipitate crystals, which
  13. filtrationwere then collected by filtration
  14. customdried

出典と根拠

ORDレコード
ord-1cba715718e34875ad2b96e5a10929bb
出典データセット
uspto-grants-1988_05
特許番号
US04746602

関連ノート

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