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Hydrochloric Acid → HCID 58734243、化合物

HRID 2080527
ノート
印刷プレビュー

反応式

HRID 2080527 の反応式
C([O:3][C:4](=[O:36])[CH2:5][S:6]([NH:9][C:10]1[CH:15]=[C:14]([CH:16]([S:25]([C:28]2[CH:33]=[CH:32][C:31]([Cl:34])=[CH:30][CH:29]=2)(=[O:27])=[O:26])[C:17]2[CH:22]=[C:21]([F:23])[CH:20]=[CH:19][C:18]=2[F:24])[C:13]([Cl:35])=[CH:12][N:11]=1)(=[O:8])=[O:7])C.O.[OH-].[Li+].Cl.FC(F)(F)C(O)=O>O1CCCC1.O.C(Cl)Cl.CO>[Cl:35][C:13]1[C:14]([CH:16]([S:25]([C:28]2[CH:33]=[CH:32][C:31]([Cl:34])=[CH:30][CH:29]=2)(=[O:27])=[O:26])[C:17]2[CH:22]=[C:21]([F:23])[CH:20]=[CH:19][C:18]=2[F:24])=[CH:15][C:10]([NH:9][S:6]([CH2:5][C:4]([OH:36])=[O:3])(=[O:8])=[O:7])=[N:11][CH:12]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 4

HCID 313Hydrochloric AcidHCID 6422Trifluoroacetic acidHCID 168937Lithium hydroxide, monohydrateHCID 58734245HCID 58734245、化合物

生成物 1

HCID 58734243HCID 58734243、化合物収率 94.2%

試薬・触媒・溶媒 4

HCID 887Methanol溶媒
HCID 962
Water
溶媒
HCID 6344Dichloromethane溶媒
HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of the ethyl[[[5-chloro-4-[(4-chlorophenylsulfonyl)(2,5-difluorophenyl)methyl]pyridin-2-yl]amino]sulfonyl]acetate (60 mg, 0.104 mmol) obtained in Example 283 in a mixture of tetrahydrofuran (5 ml) and water (1 ml) was added lithium hydroxide monohydrate (9.1 mg, 0.218 mmol). The resulting mixture was stirred at room temperature for 2 hours. To the reaction mixture was added 1N hydrochloric acid. The resulting mixture was extracted with methylene chloride. The extract was dried over anhydrous sodium sulfate, and filtered. The filtrate was concentrated under reduced pressure. The residue thus obtained was subjected to silica gel column chromatography. The fraction obtained from the methanol:methylene chloride (=1:30) eluate containing 0.5% trifluoroacetic acid was concentrated under reduced pressure to give the title compound (54 mg, 0.098 mmol, 94%) as a white solid.

後処理

  1. extractionThe resulting mixture was extracted with methylene chloride
  2. dry with materialThe extract was dried over anhydrous sodium sulfate
  3. filtrationfiltered
  4. concentrationThe filtrate was concentrated under reduced pressure
  5. customThe residue thus obtained
  6. concentrationwas concentrated under reduced pressure

出典と根拠

ORDレコード
ord-4306c06b66e54fdb8d8cdfaff6fafe9f
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

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