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Diethanolamine → 2,2'-[[6-(1H-benzimidazol-1-yl)-9H-purin-2-yl]imino]bisethanol

HRID 1453570
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인쇄 미리보기

반응식

HRID 1453570 반응식
[N:1]1([C:10]2[N:18]=[C:17](Cl)[N:16]=[C:15]3[C:11]=2[N:12]=[CH:13][NH:14]3)[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[CH:2]1.[NH:20]([CH2:24][CH2:25][OH:26])[CH2:21][CH2:22][OH:23]>CS(C)=O>[N:1]1([C:10]2[N:18]=[C:17]([N:20]([CH2:24][CH2:25][OH:26])[CH2:21][CH2:22][OH:23])[N:16]=[C:15]3[C:11]=2[N:12]=[CH:13][NH:14]3)[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[CH:2]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 8113DiethanolamineHCID 178478376HCID 178478376, 화합물

생성물 1

HCID 1785213232,2'-[[6-(1H-benzimidazol-1-yl)-9H-purin-2-yl]imino]bisethanol수율 7,042.7%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

반응 조건

온도
120 °C

실험 절차

200 mg of product obtained in stage 1 above are mixed with 3 ml of DMSO and 0.388 mg (5 equivalents) of diethanolamine, and the mixture is then heated at 120° C. for approximately 48 hours. The mixture is allowed to return to ambient temperature. Purification is carried out by chromatography on silica with a CH2Cl2-MeOH—NH4OH: 90-9-1 mixture for eluent. Evaporation is carried out and a paste is formed in methylene chloride. Partial drying and drying under vacuum at 50° C. are carried out. 88.2 mg of expected product are obtained.

후처리

  1. customto return to ambient temperature
  2. customPurification
  3. customEvaporation
  4. customa paste is formed in methylene chloride
  5. customPartial drying
  6. customdrying under vacuum at 50° C.

출처 및 근거

ORD 기록
ord-2320affbd00c44ea82df282fee9937ca
출처 데이터셋
uspto-grants-2009_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07476670B2

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