Diisopropylethylamine → HCID 10110753, 화합물

HRID 860177노트

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HRID 860177 반응식
[CH2:1]([O:8][C:9](=[O:20])[CH:10]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[C:11]([OH:13])=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl.[C:22]([C:25]1[CH:31]=[CH:30][C:28]([NH2:29])=[CH:27][CH:26]=1)(=[NH:24])[NH2:23].[B-](F)(F)(F)F.CCOC(C(C#N)=NOC(N(C)C)=[N+](C)C)=O.CCN(C(C)C)C(C)C>CN(C=O)C>[CH2:1]([O:8][C:9](=[O:20])[CH:10]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[C:11]([NH:29][C:28]1[CH:30]=[CH:31][C:25]([C:22](=[NH:23])[NH2:24])=[CH:26][CH:27]=1)=[O:13])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

6

반응물 4

HCID 81531DiisopropylethylamineHCID 117278Propanedioic acid, 2-phenyl-, 1-(phenylmethyl) esterHCID 122765Benzenecarboximidamide, 4-amino-, hydrochloride (1:1)HCID 2733286O-[(Ethoxycarbonyl)cyanomethylenamino]-N,N,N',N'-tetramethyluronium tetrafluoroborate

생성물 1

HCID 10110753HCID 10110753, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
0 °C

실험 절차

10 g (37 mmol) phenyl malonic acid monobenzyl ester and 7.7 g (37 mmol) 4-amidino aniline hydrochloride were dissolved in 60 ml DMF and cooled to 0° C. 12.2 g (37 mmol) TOTU and 19 ml (111 mmol) DIPEA were added and the mixture stirred at rt overnight. The solvent was removed, the residue taken up in ethyl acetate, and extracted with 10% sodium carbonate solution and brine. After drying over sodium sulfate, the solution was evaporated to dryness and extracted with diethyl ether twice. The remaining solid product was sufficiently pure.

후처리

  1. customThe solvent was removed
  2. extractionextracted with 10% sodium carbonate solution and brine
  3. dry with materialAfter drying over sodium sulfate
  4. customthe solution was evaporated to dryness
  5. extractionextracted with diethyl ether twice

출처 및 근거

ORD 기록
ord-c428ea3bc47b4a69b4669247d5a38618
출처 데이터셋
uspto-grants-2006_12
특허 번호
US07153876B2

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