Diisopropylethylamine → HCID 131723228, 화합물

HRID 1937814노트

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HRID 1937814 반응식
[C:1]([C:3]1[CH:18]=[CH:17][C:6]([CH2:7][CH:8]([C:12]([N:14]([CH3:16])[CH3:15])=[O:13])[C:9]([OH:11])=O)=[CH:5][CH:4]=1)#[N:2].[CH3:19][O:20][C:21]([C@@H:23]([NH2:30])[CH:24]1[CH2:29][CH2:28][CH2:27][CH2:26][CH2:25]1)=[O:22].Cl.[B-](F)(F)(F)F.CCOC(C(C#N)=NOC(N(C)C)=[N+](C)C)=O.C(N(C(C)C)CC)(C)C>CN(C)C=O>[CH3:19][O:20][C:21](=[O:22])[C@@H:23]([NH:30][C:9](=[O:11])[CH:8]([C:12](=[O:13])[N:14]([CH3:16])[CH3:15])[CH2:7][C:6]1[CH:5]=[CH:4][C:3]([C:1]#[N:2])=[CH:18][CH:17]=1)[CH:24]1[CH2:25][CH2:26][CH2:27][CH2:28][CH2:29]1

참가 물질

6

반응물 4

HCID 81531DiisopropylethylamineHCID 2733286O-[(Ethoxycarbonyl)cyanomethylenamino]-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 17747951(S)-Methyl 2-amino-2-cyclohexylacetate hydrochlorideHCID 22667660HCID 22667660, 화합물

생성물 1

HCID 131723228HCID 131723228, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
-10 °C

실험 절차

2-(R,S)-(4-Cyano-benzyl)-N,N-dimethyl-malonamic acid (10 g, 40.6 mmol) and L-cyclohexylglycine methylester hydrochloride (8.3 g, 40 mmol) were dissolved in dimethylformamide (500 ml). After cooling to −10° C. TOTU (13.1 g, 40 mmol) and diisopropylethylamine (10.34 g, 80 mmol) were added. The mixture was stirred for 1 hour and then allowed to warm to room temperature. After evaporation ethyl acetate was added to the residue and the organic layer was extracted with aqueous sodium hydogen carbonate solution, potassium hydrogen sulfate solution and water. The organic layer was evaporated. Yield: 14.53 g (90%); MS m/z: 400.3 (M+H)+.

후처리

  1. temperatureto warm to room temperature
  2. customAfter evaporation ethyl acetate
  3. additionwas added to the residue
  4. extractionthe organic layer was extracted with aqueous sodium hydogen carbonate solution, potassium hydrogen sulfate solution and water
  5. customThe organic layer was evaporated

출처 및 근거

ORD 기록
ord-6da3d8a95b41443bbc9f7fa99ce9cd3b
출처 데이터셋
uspto-grants-2002_05
특허 번호
US06395737B1

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