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Triethylamine → HCID 58137447、化合物

HRID 1258507
ノート
印刷プレビュー

反応式

HRID 1258507 の反応式
FC(F)(F)C(O)=O.[NH2:8][C:9]1[CH:10]=[C:11]([C:21](=[O:23])[CH3:22])[CH:12]=[C:13]([S:15]([F:20])([F:19])([F:18])([F:17])[F:16])[CH:14]=1.C(N(CC)CC)C.[CH3:31][S:32](Cl)(=[O:34])=[O:33].C(=O)([O-])O.[Na+]>C(Cl)Cl.O.C(OCC)(=O)C>[CH3:31][S:32]([N:8]([S:32]([CH3:31])(=[O:34])=[O:33])[C:9]1[CH:10]=[C:11]([C:21](=[O:23])[CH3:22])[CH:12]=[C:13]([S:15]([F:20])([F:16])([F:17])([F:18])[F:19])[CH:14]=1)(=[O:34])=[O:33]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 8471TriethylamineHCID 31297Methanesulfonyl chloride2 回HCID 516892Sodium BicarbonateHCID 86650835HCID 86650835、化合物

生成物 1

HCID 58137447HCID 58137447、化合物

試薬・触媒・溶媒 3

HCID 962Water溶媒
HCID 6344
Dichloromethane
溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

1-[3-Amino-5-(pentafluorosulfanyl)phenyl]ethanone trifluoroacetic acid salt (100 mg, example 4d) was dissolved in methylene chloride (10 ml), triethylamine (120 μl) was added, and methanesulfonyl chloride (21 μl) was added while stirring. After 2 h, the mixture was left to stand overnight and then further methanesulfonyl chloride (20 μl) was added. After a further 2 h, the solvent was drawn off and the residue was taken up with ethyl acetate and water, and adjusted to pH 9 with saturated sodium hydrogencarbonate solution, and the aqueous phase was extracted twice more with ethyl acetate. The combined extracts were dried over magnesium sulfate, filtered and concentrated. The residue was purified by means of preparative HPLC. The product-containing fractions were combined, freed of the acetonitrile and freeze-dried. 36 mg of the title compound were obtained.

後処理

  1. waitthe mixture was left
  2. waitto stand overnight
  3. waitAfter a further 2 h
  4. extractionthe aqueous phase was extracted twice more with ethyl acetate
  5. dry with materialThe combined extracts were dried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customThe residue was purified by means of preparative HPLC
  9. customfreeze-dried

出典と根拠

ORDレコード
ord-e919a7fd315e4119b2df77dee2c99250
出典データセット
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08466169B2

反応ノート

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