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Hydrochloric Acid → HCID 25122001, 화합물

HRID 383640
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HRID 383640 반응식
[CH2:1]([O:3][C:4]([NH:6][C:7]1[CH:8]=[C:9]([CH:27]=[CH:28][CH:29]=1)[CH2:10][N:11]1[C:16](=[O:17])[CH:15]=[CH:14][C:13]([C:18]2[CH:19]=[C:20]([CH:24]=[CH:25][CH:26]=2)[C:21](O)=[O:22])=[N:12]1)=[O:5])[CH3:2].Cl>C1COCC1>[CH2:1]([O:3][C:4](=[O:5])[NH:6][C:7]1[CH:29]=[CH:28][CH:27]=[C:9]([CH2:10][N:11]2[C:16](=[O:17])[CH:15]=[CH:14][C:13]([C:18]3[CH:26]=[CH:25][CH:24]=[C:20]([CH2:21][OH:22])[CH:19]=3)=[N:12]2)[CH:8]=1)[CH3:2]
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참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 59406753HCID 59406753, 화합물

생성물 1

HCID 25122001HCID 25122001, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
0 °C

실험 절차

2 g (5.1 mmol) of 3-[1-(3-ethoxycarbonylaminobenzyl)-6-oxo-1,6-dihydropyridazin-3-yl]benzoic acid are suspended in 60 ml of THF, and 12.7 ml (12.7 mmol) of borane/THF complex (1M) are added dropwise under a nitrogen atmosphere with ice-cooling. The mixture is stirred at 0° C. for 15 h. 6 ml of 2N HCl are added to the reaction mixture, which is then stirred at room temperature for 12 h. The reaction mixture is evaporated, the residue is dissolved in ethyl acetate, dried over sodium sulfate and evaporated. The product is purified by means of preparative HPLC.

후처리

  1. addition12.7 ml (12.7 mmol) of borane/THF complex (1M) are added dropwise under a nitrogen atmosphere with ice-
  2. temperaturecooling
  3. stirringis then stirred at room temperature for 12 h
  4. customThe reaction mixture is evaporated
  5. dissolutionthe residue is dissolved in ethyl acetate
  6. dry with materialdried over sodium sulfate
  7. customevaporated
  8. customThe product is purified by means of preparative HPLC

출처 및 근거

ORD 기록
ord-4dfee3264a614471800f45e93a814311
출처 데이터셋
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08367668B2

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