2,4-Dihydroxybenzaldehyde → HCID 135925163、化合物

HRID 1294727ノート

反応式

HRID 1294727 の反応式
[C:1]1([NH:11][C:12](=[S:15])[NH:13][NH2:14])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1.[OH:16][C:17]1[CH:24]=[C:23]([OH:25])[CH:22]=[CH:21][C:18]=1[CH:19]=O.S(NN)(C1C=CC(C)=CC=1)(=O)=O>CN(C)C=O>[OH:16][C:17]1[CH:24]=[C:23]([OH:25])[CH:22]=[CH:21][C:18]=1[CH:19]=[N:14][NH:13][C:12]([NH:11][C:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1)=[S:15]

参加物

5

反応物 3

HCID 72132,4-DihydroxybenzaldehydeHCID 15303P-ToluenesulfonylhydrazideHCID 2760175N-(Naphthalen-1-yl)hydrazinecarbothioamide

生成物 1

HCID 135925163HCID 135925163、化合物収率 18%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of 4-(naphth-1-yl)-3-thiosemicarbazide (26 mg, 0.12 mmol) and 2,4-dihydroxybenzaldehyde (20 mg, 0.144 mmol) in dimethylformamide (1 mL) was shaken with 4 Å molecular sieves for 60 h. PS-TsNHNH2 resin (29 mg, 0.085 mmol) was added and shaking continued for 40 h, then the resin was filtered off. The solvent was removed under vacuum and the residue dissolved in ethanol. The solvent was again removed and the process repeated to give the title compound (7 mg, 18%) as a solid. MS (ES−) m/e 336 [M−H]−.

後処理

  1. filtrationthe resin was filtered off
  2. customThe solvent was removed under vacuum
  3. dissolutionthe residue dissolved in ethanol
  4. customThe solvent was again removed

出典と根拠

ORDレコード
ord-04770624d24a4cfcaa7a5d63608e18cf
出典データセット
uspto-grants-2007_07
特許番号
US07241783B2

反応ノート

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