Triethylamine → 1-(4'-Fluorobiphenyl-4-sulfonylamino)cyclopentanecarboxylic acid benzyl ester

HRID 1872218

反応式

HRID 1872218 の反応式
C1(C)C=CC(S(O)(=O)=O)=CC=1.[CH2:12]([O:19][C:20]([C:22]1([NH2:27])[CH2:26][CH2:25][CH2:24][CH2:23]1)=[O:21])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.C(N(CC)CC)C.[F:35][C:36]1[CH:41]=[CH:40][C:39]([C:42]2[CH:47]=[CH:46][C:45]([S:48](Cl)(=[O:50])=[O:49])=[CH:44][CH:43]=2)=[CH:38][CH:37]=1>O.O1CCOCC1>[CH2:12]([O:19][C:20]([C:22]1([NH:27][S:48]([C:45]2[CH:44]=[CH:43][C:42]([C:39]3[CH:40]=[CH:41][C:36]([F:35])=[CH:37][CH:38]=3)=[CH:47][CH:46]=2)(=[O:49])=[O:50])[CH2:23][CH2:24][CH2:25][CH2:26]1)=[O:21])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1

参加物

6

反応物 3

HCID 8471TriethylamineHCID 254983Benzyl 1-aminocyclopentanecarboxylate 4-methylbenzenesulfonateHCID 27947494'-Fluorobiphenyl-4-sulfonyl chloride

生成物 1

HCID 154800081-(4'-Fluorobiphenyl-4-sulfonylamino)cyclopentanecarboxylic acid benzyl ester

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 312751,4-Dioxane溶媒

実験手順

To a solution of 1-aminocyclopentanecarboxylic acid benzyl ester p-toluenesulfonic acid salt (12.1 grams, 30.9 mmol) and triethylamine (10.0 mL, 72 mmol) in water (150 mL) and 1,4-dioxane (150 mL) was added 4'-fluorobiphenyl-4-sulfonyl chloride (8.8 grams, 32.5 mmol). The mixture was stirred at room temperature for 16 hours and then most of the solvent was removed by evaporation under vacuum. The mixture was diluted with ethyl acetate and was washed successively with dilute hydrochloric acid solution, water, and brine. The solution was dried over magnesium sulfate and concentrated to leave 1-(4'-fluorobiphenyl-4-sulfonylamino)cyclopentanecarboxylic acid benzyl ester as a solid, 12.33 grams (76%).

後処理

  1. custommost of the solvent was removed by evaporation under vacuum
  2. additionThe mixture was diluted with ethyl acetate
  3. washwas washed successively with dilute hydrochloric acid solution, water, and brine
  4. dry with materialThe solution was dried over magnesium sulfate
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-8057c7a85fb74f4fa79730d812f72cd6
出典データセット
uspto-grants-2000_08
特許番号
US06107337

関連ノート

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