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Sodium Iodide → HCID 19786585、化合物

HRID 1196584
ノート
印刷プレビュー

反応式

HRID 1196584 の反応式
Cl[CH2:2][CH2:3][CH2:4][CH:5]1[C:19](=[O:20])[C:9]2[C:10]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)=[N:11][O:12][C:8]=2[CH2:7][CH2:6]1.C(N(C(C)C)CC)(C)C.[O:30]=[C:31]1[N:35]([CH:36]2[CH2:41][CH2:40][NH:39][CH2:38][CH2:37]2)[C:34]2[CH:42]=[CH:43][CH:44]=[CH:45][C:33]=2[NH:32]1.[I-].[Na+]>C(OCC)(=O)C.O.CN(C=O)C>[O:30]=[C:31]1[N:35]([CH:36]2[CH2:37][CH2:38][N:39]([CH2:2][CH2:3][CH2:4][CH:5]3[C:19](=[O:20])[C:9]4[C:10]([C:13]5[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=5)=[N:11][O:12][C:8]=4[CH2:7][CH2:6]3)[CH2:40][CH2:41]2)[C:34]2[CH:42]=[CH:43][CH:44]=[CH:45][C:33]=2[NH:32]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 5238Sodium IodideHCID 81531DiisopropylethylamineHCID 886381,3-Dihydro-1-(4-piperidinyl)-2H-benzimidazol-2-oneHCID 19786584HCID 19786584、化合物

生成物 1

HCID 19786585HCID 19786585、化合物収率 27.9%

試薬・触媒・溶媒 3

HCID 962Water
溶媒
HCID 6228Dimethylformamide溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
78 °C

実験手順

To a solution consisting of 5-(3-chloropropyl)-6,7-dihydro-3-phenyl-1,2-benzisoxazol-4(5H)-one (4.19 g) and DMF (150 ml) was added diisopropylethyl amine (6.31 ml), 4-(2-keto-1-benzimidazolinyl)piperidine (3.46 g) and sodium iodide (2.17 g) at room temperature with stirring. The reaction was heated at 78° C. under nitrogen atmosphere with stirring (11 hours). Upon cooling to room temperature, water and ethyl acetate were added to the reaction mixture. The layers were separated and the aqueous layer extracted three times with ethyl acetate and once with ether. The combined organic layers were washed with brine and dried (MgSO4). Filtration and concentration gave the crude product. Purification via flash chromatography (silica gel, 1% methanol/2% Et3N/ether) afforded 1.90 g of 6,7-dihydro-5-[3-(4-(2-keto-1-benzimidazolinyl)-1-piperidinyl)-propyl]-3-phenyl-1,2-benzisoxazol-4(5H)-one, m.p. 212°-218° C.

後処理

  1. stirringwith stirring (11 hours)
  2. temperatureUpon cooling to room temperature
  3. customThe layers were separated
  4. extractionthe aqueous layer extracted three times with ethyl acetate
  5. washThe combined organic layers were washed with brine
  6. dry with materialdried (MgSO4)
  7. filtrationFiltration and concentration
  8. customgave the crude product
  9. customPurification via flash chromatography (silica gel, 1% methanol/2% Et3N/ether)

出典と根拠

ORDレコード
ord-730c6009cc5a403495e11d598c95c582
出典データセット
uspto-grants-1992_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05114936

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート