1,2-Dichloroethane → HCID 86679499, 화합물

HRID 1776543노트

반응식

HRID 1776543 반응식
[NH2:1][C:2](=[O:20])[CH2:3][N:4]([C:9]1[CH:10]=[C:11]([CH:15]=[CH:16][C:17]=1[O:18][CH3:19])[C:12]([OH:14])=[O:13])[S:5]([CH3:8])(=[O:7])=[O:6].O[CH2:22][C:23]([O:25][CH2:26][C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1)=[O:24].C(Cl)CCl>CN(C1C=CN=CC=1)C.CN(C=O)C.O>[NH2:1][C:2](=[O:20])[CH2:3][N:4]([C:9]1[CH:10]=[C:11]([CH:15]=[CH:16][C:17]=1[O:18][CH3:19])[C:12]([O:14][CH2:22][C:23]([O:25][CH2:26][C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1)=[O:24])=[O:13])[S:5]([CH3:8])(=[O:7])=[O:6]

참가 물질

7

반응물 3

HCID 111,2-DichloroethaneHCID 561337Benzyl 2-hydroxyacetateHCID 86679498HCID 86679498, 화합물

생성물 1

HCID 86679499HCID 86679499, 화합물수율 81%

시약·촉매·용매 3

HCID 142844-(Dimethylamino)pyridine촉매HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

3-(N-(2-amino-2-oxoethyl)methylsulfonamido)-4-methoxybenzoic acid (150 mg, 0.496 mmol), benzyl 2-hydroxyacetate (165 mg, 0.992 mmol), DMAP (121 mg, 0.992 mmol), and EDC (285 mg, 1.489 mmol) were dissolved in DMF (2 ml). The reaction was stirred at RT for 3 h to achieve completion. The reaction mixture was diluted with water, and extracted with EtOAc. The organic phase was washed with HCl 1N, Na2CO3 sat. sol. and brine, dried over Na2SO4 and concentrated under vacuum to give 2-(benzyloxy)-2-oxoethyl 3-(N-(2-amino-2-oxoethyl)-methylsulfonamido)-4-methoxybenzoate (180 mg, 81% yield).

후처리

  1. extractionextracted with EtOAc
  2. washThe organic phase was washed with HCl 1N, Na2CO3 sat. sol. and brine
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-882cfa363c0041efb13a69dfa6b8f51f
출처 데이터셋
uspto-grants-2016_02
특허 번호
US09265768B2

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