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Tetrahydrofuran → HCID 23114738、化合物

HRID 2080525
ノート
印刷プレビュー

反応式

HRID 2080525 の反応式
O1CCCC1.C([O:8][C:9](=O)[CH2:10][S:11]([NH:14][C:15]1[CH:20]=[C:19]([CH:21]([S:30]([C:33]2[CH:38]=[CH:37][C:36]([Cl:39])=[CH:35][CH:34]=2)(=[O:32])=[O:31])[C:22]2[CH:27]=[C:26]([F:28])[CH:25]=[CH:24][C:23]=2[F:29])[C:18]([Cl:40])=[CH:17][N:16]=1)(=[O:13])=[O:12])C.[H-].[Al+3].[Li+].[H-].[H-].[H-].[Cl-].[NH4+]>CCCCCC.CCOCC>[Cl:40][C:18]1[C:19]([CH:21]([S:30]([C:33]2[CH:34]=[CH:35][C:36]([Cl:39])=[CH:37][CH:38]=2)(=[O:32])=[O:31])[C:22]2[CH:27]=[C:26]([F:28])[CH:25]=[CH:24][C:23]=2[F:29])=[CH:20][C:15]([NH:14][S:11]([CH2:10][CH2:9][OH:8])(=[O:13])=[O:12])=[N:16][CH:17]=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

7

反応物 4

HCID 8028TetrahydrofuranHCID 25517Ammonium ChlorideHCID 21226445Aluminium lithium hydrideHCID 58734245HCID 58734245、化合物

生成物 1

HCID 23114738HCID 23114738、化合物収率 63%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether
溶媒
HCID 8058Hexane溶媒

反応条件

温度
0 °C

実験手順

To a tetrahydrofuran (5 ml) solution of ethyl[[[5-chloro-4-[(4-chlorophenylsulfonyl)(2,5-difluorophenyl)methyl]pyridin-2-yl]amino]sulfonyl]acetate (67 mg, 0.116 mmol) was added an ether solution (0.18 ml) of 1M lithium aluminum hydride at 0° C. The resulting mixture was stirred at 0° C. After the termination of the reaction was confirmed by TLC, a saturated aqueous solution of ammonium chloride was added to the reaction mixture. The resulting mixture was filtered through Celite. The filtrate was dried over anhydrous sodium sulfate, and filtered. The filtrate was concentrated under reduced pressure. The residue thus obtained was subjected to flash silica gel column chromatography. The fraction obtained from the hexane:ethyl acetate (=2:1) eluate was concentrated under reduced pressure to give the title compound (39 mg, 0.073 mmol, 63%) as a white solid.

後処理

  1. filtrationThe resulting mixture was filtered through Celite
  2. dry with materialThe filtrate was dried over anhydrous sodium sulfate
  3. filtrationfiltered
  4. concentrationThe filtrate was concentrated under reduced pressure
  5. customThe residue thus obtained
  6. concentrationethyl acetate (=2:1) eluate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-b5f6d5d6551a4ffea34dfe6f30d76ec9
出典データセット
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07932271B2

反応ノート

読み込み中…

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