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Diisopropylethylamine → HCID 66898996, 화합물

HRID 19312
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HRID 19312 반응식
[Cl:1][C:2]1[CH:23]=[CH:22][CH:21]=[CH:20][C:3]=1[O:4][C:5]1[CH2:9][N:8]([C@@H:10]([CH2:14][C:15]([F:18])([F:17])[CH3:16])[C:11]([OH:13])=O)[C:7](=[O:19])[CH:6]=1.[CH3:24][C:25]1([CH3:37])[O:29][C@H:28]([CH2:30][N:31]2[CH:35]=[CH:34][C:33]([NH2:36])=[N:32]2)[CH2:27][O:26]1.C(N(CC)C(C)C)(C)C.F[P-](F)(F)(F)(F)F.N1(O[P+](N(C)C)(N(C)C)N(C)C)C2C=CC=CC=2N=N1>CN(C)C=O.C(OCC)(=O)C>[CH3:24][C:25]1([CH3:37])[O:29][C@H:28]([CH2:30][N:31]2[CH:35]=[CH:34][C:33]([NH:36][C:11](=[O:13])[C@@H:10]([N:8]3[CH2:9][C:5]([O:4][C:3]4[CH:20]=[CH:21][CH:22]=[CH:23][C:2]=4[Cl:1])=[CH:6][C:7]3=[O:19])[CH2:14][C:15]([F:18])([F:17])[CH3:16])=[N:32]2)[CH2:27][O:26]1
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참가 물질

7

반응물 4

HCID 81531DiisopropylethylamineHCID 151348Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphateHCID 59344941(R)-1-((2,2-Dimethyl-1,3-dioxolan-4-yl)methyl)-1H-pyrazol-3-amineHCID 66894718HCID 66894718, 화합물

생성물 1

HCID 66898996HCID 66898996, 화합물수율 40.3%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매
HCID 8857Ethyl Acetate용매

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온도
25 °C

실험 절차

A solution of (S)-2-[4-(2-chloro-phenoxy)-2-oxo-2,5-dihydro-pyrrol-1-yl]-4,4-difluoro-pentanoic acid (117 mg, 0.34 mmol) and 1-((R)-2,2-dimethyl-[1,3]dioxolan-4-yl-methyl)-1H-pyrazol-3-ylamine (prepared as in Example 49, 82 mg, 0.42 mmol) in N,N-dimethylformamide (3 mL) was treated with N,N-diisopropyethylamine (170 μL, 1.02 mmol) and (benzotriazol-1-yloxy)tris(dimethylamino)phosphonium hexafluorophosphate (225 mg, 0.51 mmol) and stirred overnight at 25° C. After this time, the mixture was diluted with ethyl acetate (25 mL) and washed with a saturated aqueous solution of ammonium chloride (25 mL), saturated aqueous solution of sodium bicarbonate (25 mL) and a saturated aqueous solution of sodium chloride (25 mL) dried over sodium sulfate and concentrated with silica gel (2 g). Purification by Biotage flash chromatography (Aspire 40 g column, 20% ethyl acetate/hexanes) afforded (S)-2-[4-(2-chloro-phenoxy)-2-oxo-2,5-dihydro-pyrrol-1-yl]-4,4-difluoro-pentanoic acid [1-((R)-2,2-dimethyl-[1,3]dioxolan-4-yl-methyl)-1H-pyrazol-3-yl]-amide (72 mg, 40%) as a white foam: HR-ES-MS m/z calculated for C24H27N4O5ClF2 [M+Na]+ 547.1530, observed 547.1531.

후처리

  1. washwashed with a saturated aqueous solution of ammonium chloride (25 mL), saturated aqueous solution of sodium bicarbonate (25 mL)
  2. dry with materiala saturated aqueous solution of sodium chloride (25 mL) dried over sodium sulfate
  3. concentrationconcentrated with silica gel (2 g)
  4. customPurification by Biotage flash chromatography (Aspire 40 g column, 20% ethyl acetate/hexanes)

출처 및 근거

ORD 기록
ord-43cab93e15c34a319d97ef3ad682f4bf
출처 데이터셋
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07741327B2

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