Diisopropylethylamine → HCID 59369701, 화합물

HRID 45400

반응식

HRID 45400 반응식
[NH2:1][C:2]1[S:3][C:4]([C:13]([NH:15][CH2:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)=[O:14])=[C:5]([CH2:7][N:8]([CH2:11][CH3:12])[CH2:9][CH3:10])[N:6]=1.C(N(C(C)C)CC)(C)C.[CH2:32]([C:39]1[CH:47]=[CH:46][C:42]([C:43](O)=[O:44])=[CH:41][CH:40]=1)[C:33]1[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=1.F[P-](F)(F)(F)(F)F.C[N+](C)=C(N(C)C)ON1C2N=CC=CC=2N=N1>ClCCl.C(OCC)(=O)C>[CH2:16]([NH:15][C:13]([C:4]1[S:3][C:2]([NH:1][C:43](=[O:44])[C:42]2[CH:41]=[CH:40][C:39]([CH2:32][C:33]3[CH:34]=[CH:35][CH:36]=[CH:37][CH:38]=3)=[CH:47][CH:46]=2)=[N:6][C:5]=1[CH2:7][N:8]([CH2:9][CH3:10])[CH2:11][CH3:12])=[O:14])[C:17]1[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=1

참가 물질

7

반응물 4

HCID 81531DiisopropylethylamineHCID 1364294-Benzylbenzoic acidHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 866425252-amino-N-benzyl-4-((diethylamino)methyl)thiazole-5-carboxamide

생성물 1

HCID 59369701HCID 59369701, 화합물수율 3.7%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 2-amino-N-benzyl-4-((diethylamino)methyl)thiazole-5-carboxamide (0.052 g, 0.16 mmol) and diisopropylethylamine (0.30 mL, 1.70 mmol) in dichloromethane (5 mL) was added 4-benzylbenzoic acid (0.046 g, 0.21 mmol) followed by the addition of N,N,N′,N′-tetramethyl-O-(7-azabenzotriazol-1-yl)uronium hexafluorophosphate (0.076 g, 0.20 mmol). The reaction mixture was stirred at ambient temperature for 18 h, diluted with ethyl acetate and washed with saturated sodium bicarbonate solution, brine, dried over anhydrous magnesium sulfate, filtered and concentrated in vacuo. The crude product was purified by preparative HPLC (acetone/water gradient) to afford the title compound (0.003 g); MS (ES+) m/z 513.

후처리

  1. washwashed with saturated sodium bicarbonate solution, brine
  2. dry with materialdried over anhydrous magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customThe crude product was purified by preparative HPLC (acetone/water gradient)

출처 및 근거

ORD 기록
ord-2767760b1be14db685a7ea992c725540
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08541457B2

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