Benzoyl chloride → HCID 59850297、化合物

HRID 1642647ノート

反応式

HRID 1642647 の反応式
[CH2:1]([C:8]1[CH:13]=[CH:12][C:11]([N:14]2[S:18](=[O:20])(=[O:19])[NH:17][C:16](=[O:21])[CH2:15]2)=[C:10]([OH:22])[CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CC([O-])(C)C.[K+].[C:29](Cl)(=[O:36])[C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1>CN(C=O)C>[CH2:1]([C:8]1[CH:13]=[CH:12][C:11]([N:14]2[CH2:15][C:16](=[O:21])[NH:17][S:18]2(=[O:20])=[O:19])=[C:10]([O:22][C:29](=[O:36])[C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=2)[CH:9]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 7412Benzoyl chlorideHCID 23665647Potassium tert-butoxideHCID 24895697HCID 24895697、化合物

生成物 1

HCID 59850297HCID 59850297、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 5-(4-benzyl-2-hydroxyphenyl)-1,1-dioxo-1,2,5-thiadiazolidin-3-one (45 mg, 0.141 mmol) in DMF (0.2 mL) is added KOtBu (1.0 M in THF, 0.17 mL, 0.17 mmol). After it is stirred at ambient temperature for 5 min., benzoyl chloride (35 mg, 0.254 mmol) is added. After it is stirred at ambient temperature for 10 min., the reaction is quenched with 1N HCl solution. The residue is then purified by prep. HPLC using CH3CN (0.1% TFA)/water (5-70%) to give the title compound: MS (M−H)−=421.

後処理

  1. stirringAfter it is stirred at ambient temperature for 10 min.
  2. customthe reaction is quenched with 1N HCl solution
  3. customThe residue is then purified by prep

出典と根拠

ORDレコード
ord-906de45988364db09f1bce0f8b8c9968
出典データセット
uspto-grants-2012_02
特許番号
US08119666B2

反応ノート

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