2,4-Dihydroxybenzaldehyde → HCID 135925163, 화합물

HRID 1294727노트

반응식

HRID 1294727 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 135925163HCID 135925163, 화합물수율 18%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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]−.

후처리

  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

출처 및 근거

ORD 기록
ord-04770624d24a4cfcaa7a5d63608e18cf
출처 데이터셋
uspto-grants-2007_07
특허 번호
US07241783B2

반응 노트

불러오는 중…