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Water → HCID 15859997、化合物

HRID 549783
ノート
印刷プレビュー

反応式

HRID 549783 の反応式
[F:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6]([CH2:13][C:14]([N:16]3[CH2:21][CH2:20][N:19]([C:22]4[C:27]5[CH:28]=[CH:29][S:30][C:26]=5[CH:25]=[CH:24][N:23]=4)[CH2:18][CH2:17]3)=O)=[CH:7][C:8](=[O:12])[NH:9]2)=[CH:4][CH:3]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>O1CCCC1>[F:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6]([CH2:13][CH2:14][N:16]3[CH2:21][CH2:20][N:19]([C:22]4[C:27]5[CH:28]=[CH:29][S:30][C:26]=5[CH:25]=[CH:24][N:23]=4)[CH2:18][CH2:17]3)=[CH:7][C:8](=[O:12])[NH:9]2)=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962Water2 回HCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 25028976HCID 25028976、化合物

生成物 1

HCID 15859997HCID 15859997、化合物収率 64.6%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒
2 回

実験手順

107.7 kg (1 eq.) of intermediate 7-fluoro-4-[2-[4-(thieno[3,2-c]pyridin-4-yl)piperazin-1-yl]-2-oxoethyl]quinolin-2(1H)-one (I), followed by 3231 of THF, are introduced, in thirty minutes at 10° C., into a suspension of 22.2 kg (2.3 eq.) of lithium aluminium hydride in 580 l of tetrahydrofuran, in a reactor. The mixture is stirred for three hours at ambient temperature and then, after verification that the reaction is complete, the mixture is cooled and 21.5 l of water, 21.5 l of 4N sodium hydroxide and 180 l of water are added successively without the temperature exceeding 15° C. The mixture is stirred for one hour and the inorganic salts are filtered off. The mixture is concentrated to three volumes of THF and run into 1400 l of water. The mixture is filtered and a paste is re-formed in 1000 l of a water/THF mixture: 3/7. The product is dried under vacuum at 50° C. Compound (V) is obtained.

後処理

  1. temperaturethe mixture is cooled
  2. customexceeding 15° C
  3. stirringThe mixture is stirred for one hour
  4. filtrationthe inorganic salts are filtered off
  5. concentrationThe mixture is concentrated to three volumes of THF
  6. filtrationThe mixture is filtered
  7. customa paste is re-formed in 1000 l of a water/THF mixture
  8. customThe product is dried under vacuum at 50° C

出典と根拠

ORDレコード
ord-8a4f2e7d28484de284e89c28b49d7f29
出典データセット
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07943769B2

反応ノート

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