Trifluoroacetic acid → HCID 55290747、化合物

HRID 2111677ノート

反応式

HRID 2111677 の反応式
FC(F)(F)C(O)=O.[OH:8][CH2:9][C:10]1[CH:14]=[C:13]([CH2:15][NH:16]C(OC(C)(C)C)=O)[O:12][N:11]=1>C(Cl)Cl>[NH3:11].[OH:8][CH2:9][C:10]1[CH:14]=[C:13]([CH2:15][NH2:16])[O:12][N:11]=1

参加物

5

反応物 2

HCID 6422Trifluoroacetic acidHCID 67284568543713-48-0

生成物 2

HCID 222AmmoniaHCID 55290747HCID 55290747、化合物収率 195.4%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Trifluoroacetic acid (4 ml, 54 mmol) was added to a solution of 3-hydroxymethyl-5-[N-(tert-butyloxycarbonyl)aminomethyl]isoxazole (Method 75; 1.25 g, 5.4 mmol) in DCM (40 ml). The mixture was stirred at ambient temperature for 18 hours then the volatiles removed by evaporation. The residue was purified by chromatography on a SCX-2 column (50 g) eluting with methanol then 7N ammonia in methanol to give the title compound (676 mg, 96%). NMR (DMSO): 1.97 (br s, 2H), 3.76 (s, 2H), 4.44 (s, 2H), 5.38 (s, 1H), 6.26 (s, 1H).

後処理

  1. customthe volatiles removed by evaporation
  2. customThe residue was purified by chromatography on a SCX-2 column (50 g)
  3. washeluting with methanol

出典と根拠

ORDレコード
ord-90c1ead4e53a4e3489884b94115bed20
出典データセット
uspto-grants-2009_04
特許番号
US07521453B2

反応ノート

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