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Diethyl Oxalate → Ethyl [2-({7-(benzyloxy)-5-[4-(methylsulfonyl)phenoxy]-1H-indol-2-yl}carbonyl)hydrazino](oxo)acetate

HRID 1188891
ノート
印刷プレビュー

反応式

HRID 1188891 の反応式
O.NN.[C:4]([O:11][CH2:12][CH3:13])(=[O:10])[C:5]([O:7]CC)=O.[CH2:14]([O:21][C:22]1[CH:23]=[C:24]([O:34][C:35]2[CH:40]=[CH:39][C:38]([S:41]([CH3:44])(=[O:43])=[O:42])=[CH:37][CH:36]=2)[CH:25]=[C:26]2[C:30]=1[NH:29][C:28]([C:31](O)=[O:32])=[CH:27]2)[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.Cl.CN(C)CCCN=C=NCC.O[N:58]1C2C=CC=CC=2N=[N:59]1>C(O)C.CCCCCC.C(OCC)(=O)C.O.CN(C)C=O>[CH2:14]([O:21][C:22]1[CH:23]=[C:24]([O:34][C:35]2[CH:36]=[CH:37][C:38]([S:41]([CH3:44])(=[O:42])=[O:43])=[CH:39][CH:40]=2)[CH:25]=[C:26]2[C:30]=1[NH:29][C:28]([C:31]([NH:58][NH:59][C:5](=[O:7])[C:4]([O:11][CH2:12][CH3:13])=[O:10])=[O:32])=[CH:27]2)[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

11

反応物 5

HCID 7268Diethyl OxalateHCID 24654Hydrazine hydrate (1:1)HCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 668975467-(Benzyloxy)-5-[4-(methylsulfonyl)phenoxy]-1H-indole-2-carboxylic acid

生成物 1

HCID 66897270
Ethyl [2-({7-(benzyloxy)-5-[4-(methylsulfonyl)phenoxy]-1H-indol-2-yl}carbonyl)hydrazino](oxo)acetate
収率 83%

試薬・触媒・溶媒 5

HCID 702Ethanol溶媒2 回HCID 962Water溶媒HCID 6228Dimethylformamide溶媒HCID 8058Hexane溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A solution of hydrazine monohydrate (0.1 mL) in ethanol (2 mL) was added dropwise to a solution of diethyl oxalate (0.3 mL) in ethanol (2 mL) under ice-cooling. The reaction mixture was concentrated under reduced pressure to give a white solid. A mixture of 7-(benzyloxy)-5-[4-(methylsulfonyl)phenoxy]-1H-indole-2-carboxylic acid (450 mg), 1-[3-(dimethylamino)propyl-3-ethylcarbodiimide hydrochloride (403 mg), 1-hydroxybenzotriazole (284 mg) and N,N-dimethylformamide (20 mL) was stirred at room temperature for 30 min, the previous-obtained white solid was added, and the mixture was stirred at room temperature for 2 hr. Water was added to the reaction solution, and the mixture was subjected to extraction with ethyl acetate. The organic layer was washed with saturated brine, dried over magnesium sulfate, filtrated, and concentrated under reduced pressure. The obtained crude product was subjected to silica gel column chromatography (ethyl acetate:hexane=20:80-90:10, volume ratio) to give the title compound (420 mg, yield 83%) as an orange oil. MS 552 (MH+).

後処理

  1. temperaturecooling
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. customto give a white solid
  4. additionthe previous-obtained white solid was added
  5. stirringthe mixture was stirred at room temperature for 2 hr
  6. extractionthe mixture was subjected to extraction with ethyl acetate
  7. washThe organic layer was washed with saturated brine
  8. dry with materialdried over magnesium sulfate
  9. filtrationfiltrated
  10. concentrationconcentrated under reduced pressure
  11. customThe obtained crude product

出典と根拠

ORDレコード
ord-2101a507ae0c47ba971d0f4dd294fd04
出典データセット
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08673942B2

反応ノート

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