Diisopropylethylamine → HCID 10110753、化合物

HRID 860177ノート

反応式

HRID 860177 の反応式
[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

参加物

6

反応物 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

生成物 1

HCID 10110753HCID 10110753、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
0 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c428ea3bc47b4a69b4669247d5a38618
出典データセット
uspto-grants-2006_12
特許番号
US07153876B2

反応ノート

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