Diisopropylethylamine → HCID 58386517, 화합물

HRID 74652

반응식

HRID 74652 반응식
[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]2[NH:12][C:11](=[O:13])[N:10]([CH:14]3[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]3)[CH2:9][CH2:8][C:7]=2[CH:20]=1.Cl[C:22]1[N:27]=[CH:26][N:25]=[C:24]([C:28]([N:30]2[CH:38]3[CH:33]([CH2:34][CH2:35][CH2:36][CH2:37]3)[CH2:32][CH2:31]2)=[O:29])[CH:23]=1.CCN(C(C)C)C(C)C>CN(C=O)C>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]2[NH:12][C:11](=[O:13])[N:10]([CH:14]3[CH2:19][CH2:18][N:17]([C:22]4[CH:23]=[C:24]([C:28]([N:30]5[CH:38]6[CH:33]([CH2:34][CH2:35][CH2:36][CH2:37]6)[CH2:32][CH2:31]5)=[O:29])[N:25]=[CH:26][N:27]=4)[CH2:16][CH2:15]3)[CH2:9][CH2:8][C:7]=2[CH:20]=1

참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 183568527-methoxy-3-(piperidin-4-yl)-4,5-dihydro-1H-benzo[d][1,3]diazepin-2(3H)-oneHCID 58386728(6-Chloropyrimidin-4-yl)-(octahydroindol-1-yl)-methanone

생성물 1

HCID 58386517HCID 58386517, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

705 mg (2.56 mmol) 7-methoxy-3-piperidin-4-yl-1,3,4,5-tetrahydro-1,3-benzodiazepin-2-one, 680 mg (2.56 mmol) (6-chloro-pyrimidin-4-yl)-(octahydro-indol-1-yl)-methanone and 0.871 mL (5 mmol) DIPEA were stirred in 10 mL DMF for 2 h at RT. The reaction mixture was purified by HPLC. The product-containing fractions were combined and the ACN was eliminated by rotary evaporation. The aqueous phase was made alkaline with 4M NaOH and extracted with EtOAc. The organic phase was dried, filtered and the filtrate was concentrated to dryness by rotary evaporation. The residue was crystallised from a mixture of MeOH and diethyl ether and the solid was suction filtered and dried.

후처리

  1. customThe reaction mixture was purified by HPLC
  2. customthe ACN was eliminated by rotary evaporation
  3. extractionextracted with EtOAc
  4. customThe organic phase was dried
  5. filtrationfiltered
  6. concentrationthe filtrate was concentrated to dryness by rotary evaporation
  7. customThe residue was crystallised from a mixture of MeOH and diethyl ether
  8. filtrationfiltered
  9. customdried

출처 및 근거

ORD 기록
ord-441a4bff0ea9403996c1db01ffb535b0
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08829006B2

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