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Hydrochloric Acid → 1-(4-Fluoro-2,3-dihydroindol-1-yl)-2-(4-methoxy-6-chloropyrimidin-2-yl)ethanone

HRID 2278531
ノート
印刷プレビュー

反応式

HRID 2278531 の反応式
[F:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]2[C:3]=1[CH2:4][CH2:5][NH:6]2.Cl.CN(C)CCCN=C=NCC.[Na].[CH3:24][O:25][C:26]1[CH:31]=[C:30]([Cl:32])[N:29]=[C:28]([CH2:33][C:34](O)=[O:35])[N:27]=1.Cl>CN(C=O)C.N1C=CC=CC=1.C(OCC)C.O.C(OCC)(=O)C>[F:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]2[C:3]=1[CH2:4][CH2:5][N:6]2[C:34](=[O:35])[CH2:33][C:28]1[N:27]=[C:26]([O:25][CH3:24])[CH:31]=[C:30]([Cl:32])[N:29]=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 313Hydrochloric AcidHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 5360545SodiumHCID 12420761(4-Chloro-6-methoxypyrimidin-2-yl)acetic acidHCID 162444404-Fluoro-2,3-dihydro-1H-indole

生成物 1

HCID 866992651-(4-Fluoro-2,3-dihydroindol-1-yl)-2-(4-methoxy-6-chloropyrimidin-2-yl)ethanone

試薬・触媒・溶媒 5

HCID 962Water溶媒HCID 1049Pyridine溶媒HCID 3283Diethyl Ether溶媒HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

3.32 g of 4-fluoro-2,3-dihydro-1H-indole and 5.56 g of N-[3-(dimethylamino)propyl]-N′-ethylcarbodiimide hydrochloride are added to a solution of 5.4 g of the sodium salt of (4-methoxy-6-chloropyrimidin-2-yl)acetic acid in 50 ml of DMF and 4.3 ml of pyridine. The reaction medium is stirred at ambient temperature for one hour. 200 ml of ethyl acetate and 100 ml of water are added, and also 1N hydrochloric acid to pH=5-6. After settling out, the organic phase is dried over magnesium sulfate, filtered, and then concentrated under reduced pressure. The oil obtained is taken up with ethyl ether. The solid formed is filtered off so as to give 2.2 g of 1-(4-fluoro-2,3-dihydroindol-1-yl)-2-(4-methoxy-6-chloropyrimidin-2-yl)ethanone in the form of an orangey-colored solid, the characteristics of which are the following:

後処理

  1. dry with materialthe organic phase is dried over magnesium sulfate
  2. filtrationfiltered
  3. concentrationconcentrated under reduced pressure
  4. customThe oil obtained
  5. customThe solid formed
  6. filtrationis filtered off so as

出典と根拠

ORDレコード
ord-89227cdda80b4de69f572f596545ec28
出典データセット
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09133168B2

反応ノート

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