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Triethylamine → HCID 67768232, 화합물

HRID 2396087
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HRID 2396087 반응식
[C:1]([O:5][C:6]([NH:8][C@@H:9]([CH2:19][S:20][C:21]([C:34]1[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=1)([C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1)[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)[CH2:10][N:11]1[CH2:18][CH2:17][CH2:16][C@H:12]1[C:13]([OH:15])=[O:14])=[O:7])([CH3:4])([CH3:3])[CH3:2].CN(C)CCCN=C=NCC.O.[OH:52]N1C2C=CC=CC=2N=N1.[Cl:62][C:63]1[C:70]([Cl:71])=[CH:69][CH:68]=[CH:67][C:64]=1[CH2:65][NH2:66].CCN(CC)CC>CN(C=O)C>[C:1]([O:5][C:6]([NH:8][C@@H:9]([CH2:19][S:20][C:21]([C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)([C:34]1[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=1)[C:28]1[CH:29]=[CH:30][CH:31]=[CH:32][CH:33]=1)[CH2:10][N:11]1[CH2:18][CH2:17][CH2:16][C@H:12]1[C:13]([OH:15])=[O:14])=[O:7])([CH3:4])([CH3:2])[CH3:3].[Cl:62][C:63]1[C:70]([Cl:71])=[CH:69][CH:68]=[CH:67][C:64]=1[C:65]([NH2:66])=[O:52]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 8471TriethylamineHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 5876252,3-DichlorobenzylamineHCID 27960291-Hydroxybenzotriazole hydrateHCID 22858731HCID 22858731, 화합물

생성물 1

HCID 67768232HCID 67768232, 화합물

시약·촉매·용매

1
HCID 6228Dimethylformamide용매

실험 절차

[2(R)-(t-butoxycarbonyl)amino-3-triphenylmethylmercaptopropyl]-L-proline (0.08 g, 0.153 mmol), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide (EDC) (0.035 g, 0.184 mmol), and 1-hydroxybenzotriazole hydrate (HOBT) (0.025 g,0.184 mmol) were dissolved in DMF (2 mL), treated with 2,3-dichlorobenzylamine (0.025 mL, 0.184 mmol), and brought to pH 7 with Et3N (0.026 mL, 0.184 mmol). After stirring at ambient temperature for 18 h the mixture was concentrated to dryness, and the residue was partitioned between EtOAc and H2O, the organic layer separated, washed with aq satd NaHCO3, brine, and dried (Na2SO4). Filtration and concentration provided the title compound. 1H NMR (CD3OD) δ 7.1-7.5 (m, 18H), 4.53 (d, 1H, J=8 Hz), 4.26 (d, 1H,J=8 Hz), 3.64-3.76 (m, 1H), 2.96-3.14 (m, 2H), 2.52-2.66 (m, 1H), 2.1-2.5 (m, 5H), 1.6-1.9 (m, 3H), 1.45 (s, 9H).

후처리

  1. concentrationwas concentrated to dryness
  2. customthe residue was partitioned between EtOAc and H2O
  3. customthe organic layer separated
  4. washwashed with aq satd NaHCO3, brine
  5. dry with materialdried (Na2SO4)
  6. filtrationFiltration and concentration

출처 및 근거

ORD 기록
ord-297c3c37e6104a51bbae0f0deb691426
출처 데이터셋
uspto-grants-1996_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05491164

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