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1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → HCID 69676422, 화합물

HRID 919616
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HRID 919616 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([NH:9][CH2:10][C:11]([OH:13])=O)[CH:5]=[C:6]([Cl:8])[CH:7]=1.C1C=CC2N(O)N=NC=2C=1.CCN=C=NCCCN(C)C.[CH3:35][CH:36]1[CH2:41][CH2:40][NH:39][CH2:38][CH:37]1[NH:42][C:43](=[O:49])[O:44][C:45]([CH3:48])([CH3:47])[CH3:46].CCN(C(C)C)C(C)C>CN(C=O)C>[Cl:8][C:6]1[CH:5]=[C:4]([NH:9][CH2:10][C:11]([N:39]2[CH2:40][CH2:41][CH:36]([CH3:35])[CH:37]([NH:42][C:43](=[O:49])[O:44][C:45]([CH3:48])([CH3:47])[CH3:46])[CH2:38]2)=[O:13])[CH:3]=[C:2]([Cl:1])[CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 13138167(3,5-Dichlorophenyl)glycineHCID 45092184HCID 45092184, 화합물

생성물 1

HCID 69676422HCID 69676422, 화합물수율 55.7%

시약·촉매·용매

1
HCID 6228Dimethylformamide용매

실험 절차

To a solution of 2-(3,5-dichlorophenylamino)acetic acid (153 mg, 0.69 mmol) in DMF (5 mL) was added HOBt (141 mg, 1.0 mmol), EDCI (201 mg, 1.0 mmol), tert-butyl 4-methylpiperidin-3-ylcarbamate (150 mg, 0.69 mmol), and DIEA (0.18 mL, 1.3 mmol) at 0° C. Then the reaction mixture was stirred at rt for 5 h, partitioned between EtOAc and water. The organic phase was separated and washed with brine, and concentrated in vacuo to yield the crude product, which was purified by column chromatography using 0-2% MeOH: DCM solvent mixture to yield the titled intermediate (160 mg, 54%) as a thick liquid. 1H NMR (400 MHz, CDCl3): δ 6.92 (s, 1H), 6.49 (s, 1H), 6.38 (s, 1H), 6.29 (s, 1H), 5.22-5.15 (m, 1H), 4.65-4.56 (m, 1H), 4.35-4.16 (m, 2H), 3.25-2.89 (m, 2H), 2.85-2.69 (m, 2H), 1.82-1.75 (m, 2H), 1.69-1.45 (m, 1H), 1.22 and 1.14 (2s, 9H), 1.05 and 0.95 (2d, J=6.8 Hz, 3H). LC-MS: m/z [M+1]=416.

후처리

  1. custompartitioned between EtOAc and water
  2. customThe organic phase was separated
  3. washwashed with brine
  4. concentrationconcentrated in vacuo
  5. customto yield the crude product, which
  6. customwas purified by column chromatography

출처 및 근거

ORD 기록
ord-06a4be527ef8494bbd61dc68665e11ee
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09273028B2

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