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Hydrochloric Acid → HCID 178527405、化合物

HRID 853138
ノート
印刷プレビュー

反応式

HRID 853138 の反応式
[CH2:1]([S:8]([N:11]([CH2:35][C:36]([F:39])([F:38])[F:37])[C@H:12]1[CH2:17][CH2:16][C@H:15]([C:18]([O:27][Si](CC)(CC)CC)([C:23]([F:26])([F:25])[F:24])[C:19]([F:22])([F:21])[F:20])[CH2:14][CH2:13]1)(=[O:10])=[O:9])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C[Si]([N-][Si](C)(C)C)(C)C.[Li+].[CH2:50](Br)[C:51]1[CH:56]=[CH:55][CH:54]=[CH:53][CH:52]=1.Cl>C1COCC1.CCOCC>[F:39][C:36]([F:37])([F:38])[CH2:35][N:11]([C@H:12]1[CH2:17][CH2:16][C@H:15]([C:18]([OH:27])([C:19]([F:22])([F:20])[F:21])[C:23]([F:24])([F:25])[F:26])[CH2:14][CH2:13]1)[S:8]([CH:1]([C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1)[CH2:50][C:51]1[CH:56]=[CH:55][CH:54]=[CH:53][CH:52]=1)(=[O:10])=[O:9]
参加物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 313Hydrochloric AcidHCID 7498Benzyl BromideHCID 2733832Lithium hexamethyldisilazaneHCID 178477575HCID 178477575、化合物

生成物 1

HCID 178527405HCID 178527405、化合物収率 105.7%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether
溶媒
HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of 50 mg (0.08 mmol) of trans benzyl-N-(2,2,2-trifluoro-ethyl)-N-[4-(2,2,2-trifluoro-1-triethylsilanyloxy-1-trifluoromethyl-ethyl)-cyclohexyl]-sulfonamide (example 30.1) in 0.5 mL of THF was cooled to −78° C. and treated with 0.11 mL of a 1M solution lithium bis(trimethylsilyl)amide in THF. The mixture was allowed to reach ca −5° C. within 30 min and treated with 0.11 mL (0.1 mmol) of benzylbromide. The mixture was stirred overnight and distributed between diluted aqueous solution of HCl and Et2O. The combined organic phases were dried over Na2SO4 and the solvent was evaporated. The residue was redissolved in MeOH and treated with 0.5 mL of a 2M solution of NaOMe in MeOH. Distribution of this solution between a saturated aqueous solution of NH4Cl and Et2O, drying of the combined organic phases over Na2SO4, evaporation and column chromatography on silica gel with heptane/EtOAc 4:1 gave 50 mg (76%) of (rac) trans 1,2-diphenyl-ethanesulfonic acid (2,2,2-trifluoro-ethyl)-[4-(2,2,2-trifluoro-1-hydroxy-1-trifluoromethyl-ethyl)-cyclohexyl]-amide as a colorless foam, MS: 590 (M−H)−.

後処理

  1. dry with materialThe combined organic phases were dried over Na2SO4
  2. customthe solvent was evaporated
  3. dissolutionThe residue was redissolved in MeOH
  4. additiontreated with 0.5 mL of a 2M solution of NaOMe in MeOH
  5. dry with materialDistribution of this solution between a saturated aqueous solution of NH4Cl and Et2O, drying of the combined organic phases over Na2SO4, evaporation and column chromatography on silica gel with heptane/EtOAc 4:1

出典と根拠

ORDレコード
ord-5fa07ce44b4843009a2109e121738289
出典データセット
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07253282B2

反応ノート

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