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Pentane → 4-Amino-5-chloro-N-[2-(diethylamino)ethyl]-2-(4-diethylamino-4-oxobutoxy)benzamide

HRID 1382978
ノート
印刷プレビュー

反応式

HRID 1382978 の反応式
CCCCC.[H-].[Na+].[NH2:8][C:9]1[C:24]([Cl:25])=[CH:23][C:12]([C:13]([NH:15][CH2:16][CH2:17][N:18]([CH2:21][CH3:22])[CH2:19][CH3:20])=[O:14])=[C:11]([OH:26])[CH:10]=1.Cl[CH2:28][CH2:29][CH2:30][C:31]([N:33]([CH2:36][CH3:37])[CH2:34][CH3:35])=[O:32]>CN(C=O)C.[Cl-].[Na+].O>[NH2:8][C:9]1[C:24]([Cl:25])=[CH:23][C:12]([C:13]([NH:15][CH2:16][CH2:17][N:18]([CH2:19][CH3:20])[CH2:21][CH3:22])=[O:14])=[C:11]([O:26][CH2:28][CH2:29][CH2:30][C:31]([N:33]([CH2:36][CH3:37])[CH2:34][CH3:35])=[O:32])[CH:10]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 8003PentaneHCID 24758Sodium hydrideHCID 24348694-Chloro-N,N-diethyl-butyramideHCID 9817332o-Desmethyl metoclopramide

生成物 1

HCID 200595024-Amino-5-chloro-N-[2-(diethylamino)ethyl]-2-(4-diethylamino-4-oxobutoxy)benzamide収率 79.8%

試薬・触媒・溶媒 2

HCID 6228
Dimethylformamide
溶媒
2 回
HCID 57417360Sodium chloride; water溶媒

実験手順

To a well-stirred suspension of pentane-washed sodium hydride (0.52 g of 60%, 3 mmole) in 3 ml dry DMF was added 4-amino-5-chloro-N-[2-(diethylamino)ethyl]-2-hydroxybenzamide (3.43 g, 12 mmoles) (prepared as in Example 53). To this was added 10 ml of DMF and the mixture was stirred at ambient temperature for 45 minutes then warmed to about 50° C. for 15 minutes whereupon 4-chloro-N,N-diethylbutyramide (1.92 g, 11 mmoles) was added. The mixture was then stirred at 60°-70° C. for 6 hours, at room temperature for 2 days and then at 60-70° C. for a further 4 hours. After cooling, the mixture was poured into 400 ml of brine and extracted with methylene chloride (4×100 ml). After combining, the organic phase was washed two times with 100 ml of 10% aqueous sodium hydroxide and brine, dried over sodium sulfate, filtered and concentrated in vacuo to give an oil (3.75 g). This was purified by flash chromatography on silica gel to give 1.64 g of the title compound as an oil.

後処理

  1. additionwas added
  2. stirringThe mixture was then stirred at 60°-70° C. for 6 hours, at room temperature for 2 days
  3. waitat 60-70° C. for a further 4 hours
  4. temperatureAfter cooling
  5. extractionextracted with methylene chloride (4×100 ml)
  6. washthe organic phase was washed two times with 100 ml of 10% aqueous sodium hydroxide and brine
  7. dry with materialdried over sodium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-50994d7caeb74b28b018db023f6c9509
出典データセット
uspto-grants-1989_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04808624

反応ノート

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