Methyl triflate → HCID 58558200、化合物

HRID 82718

反応式

HRID 82718 の反応式
[NH2:1][C:2]1[C:3]([C:7](=[S:17])[NH:8][C:9]2[CH:14]=[CH:13][C:12]([F:15])=[C:11]([Br:16])[CH:10]=2)=[N:4][S:5][N:6]=1.F[C:19](F)(F)S(OC)(=O)=O.C(N(CC)C(C)C)(C)C>ClCCl>[NH2:1][C:2]1[C:3]([C:7]([S:17][CH3:19])=[N:8][C:9]2[CH:14]=[CH:13][C:12]([F:15])=[C:11]([Br:16])[CH:10]=2)=[N:4][S:5][N:6]=1

参加物

5

反応物 3

HCID 9526Methyl triflateHCID 81531DiisopropylethylamineHCID 585583094-amino-N-(3-bromo-4-fluorophenyl)-1,2,5-thiadiazole-3-carbothioamide

生成物 1

HCID 58558200HCID 58558200、化合物収率 98%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of 4-amino-N-(3-bromo-4-fluorophenyl)-1,2,5-thiadiazole-3-carbothioamide (130 mg, 0.4 mmol) in dichloromethane (5.2 mL) was treated with methyl trifluoromethanesulfonate (64 μL, 0.6 mmol) followed by N,N-diisopropylethylamine (102 μL, 0.6 mmol) and stirred for 1 h. The reaction mixture was diluted with dichloromethane (100 mL), washed with water (50 mL) and brine (50 mL), dried with sodium sulfate, filtered, and concentrated to give the desired product (133 mg, 98%). LCMS for C10H9BrFN4S2 (M+H)+: m/z=346.8, 348.8.

後処理

  1. washwashed with water (50 mL) and brine (50 mL)
  2. dry with materialdried with sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-2d1203d754da490684a27a1c8980cbde
出典データセット
uspto-grants-2014_09
特許番号
US08846726B2

関連ノート

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