1,2-Dichloroethane → HCID 131721221, 화합물

HRID 1068411노트

반응식

HRID 1068411 반응식
Cl.[CH3:2][O:3][C:4](=[O:19])[C:5]1([CH2:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=2[CH3:18])[CH2:10][CH2:9][NH:8][CH2:7][CH2:6]1.[C:20]1([C:26]([C:51]2[CH:56]=[CH:55][CH:54]=[CH:53][CH:52]=2)([C:45]2[CH:50]=[CH:49][CH:48]=[CH:47][CH:46]=2)[N:27]2[CH:31]=[C:30]([CH:32]([CH2:36][C:37]3[CH:42]=[CH:41][C:40]([C:43]#[N:44])=[CH:39][CH:38]=3)[C:33](O)=[O:34])[N:29]=[CH:28]2)[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1.C1C=C2C(N(O)N=NC2=CC=1)=O.C(N(CC)CC)C.C(Cl)CCl>CN(C=O)C.CCOC(C)=O>[CH3:2][O:3][C:4](=[O:19])[C:5]1([CH2:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=2[CH3:18])[CH2:6][CH2:7][N:8]([C:33](=[O:34])[CH:32]([C:30]2[N:29]=[CH:28][N:27]([C:26]([C:51]3[CH:52]=[CH:53][CH:54]=[CH:55][CH:56]=3)([C:45]3[CH:46]=[CH:47][CH:48]=[CH:49][CH:50]=3)[C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)[CH:31]=2)[CH2:36][C:37]2[CH:38]=[CH:39][C:40]([C:43]#[N:44])=[CH:41][CH:42]=2)[CH2:9][CH2:10]1

참가 물질

8

반응물 5

HCID 111,2-DichloroethaneHCID 8471TriethylamineHCID 730263-hydroxy-1,2,3-benzotriazin-4(3H)-oneHCID 21193379HCID 21193379, 화합물HCID 21193404HCID 21193404, 화합물

생성물 1

HCID 131721221HCID 131721221, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

To a mixture of 4-(2-methylbenzyl)-isonipecotic acid methyl ester hydrochloride (72 mg, 0.25 mmol), and 2-{1-(triphenylmethyl)-1H-imidazol-4-yl}-2-(4-cyanobenzyl)-acetic acid(123 mg, 0.25 mmol), HOOBT (42 mg, 0.25 mmol) and triethylamine (0.088 ml, 0.636 mmol) in DMF (3 ml), was added EDC (54 mg, 0.25 mmol) and the reaction stirred at room temperature for 18 hrs. The reaction was diluted with EtOAc and washed with saturated NaHCO3 solution, the organic extracts were dried (Na2SO4), and the solvent evaporated in vacuo. The residue was purified by chromatography(SiO2, gradient elution, 1-5% MeOH in CH2Cl2) to afford the product.

후처리

  1. washwashed with saturated NaHCO3 solution
  2. dry with materialthe organic extracts were dried (Na2SO4)
  3. customthe solvent evaporated in vacuo
  4. customThe residue was purified by chromatography(SiO2, gradient elution, 1-5% MeOH in CH2Cl2)
  5. customto afford the product

출처 및 근거

ORD 기록
ord-2804c1c4af6c41b1baf1b4eb82a49c4d
출처 데이터셋
uspto-grants-2001_06
특허 번호
US06248756B1

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