1,2-Dichloroethane → HCID 67365779, 화합물

HRID 42833

반응식

HRID 42833 반응식
N#N.[C:3]1([C:9]2[O:13][CH:12]=[N:11][C:10]=2[C:14]([OH:16])=O)[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.C1C=CC2N(O)N=NC=2C=1.C(Cl)CCl.[C:31]([Si:35]([CH3:52])([CH3:51])[O:36][CH:37]([C:39]1[O:40][C:41]([CH2:44][N:45]2[N:49]=[C:48]([NH2:50])[CH:47]=[N:46]2)=[CH:42][N:43]=1)[CH3:38])([CH3:34])([CH3:33])[CH3:32]>C(Cl)Cl.CN(C1C=CN=CC=1)C.O>[C:31]([Si:35]([CH3:52])([CH3:51])[O:36][CH:37]([C:39]1[O:40][C:41]([CH2:44][N:45]2[N:49]=[C:48]([NH:50][C:14]([C:10]3[N:11]=[CH:12][O:13][C:9]=3[C:3]3[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=3)=[O:16])[CH:47]=[N:46]2)=[CH:42][N:43]=1)[CH3:38])([CH3:34])([CH3:33])[CH3:32]

참가 물질

9

반응물 5

HCID 111,2-DichloroethaneHCID 947NitrogenHCID 757711-HydroxybenzotriazoleHCID 27762995-Phenyl-1,3-oxazole-4-carboxylic acidHCID 673660512-{2-[1-(tert-Butyl-dimethyl-silanyloxy)-ethyl]-oxazol-5-ylmethyl}-2H-[1,2,3]triazol-4-ylamine

생성물 1

HCID 67365779HCID 67365779, 화합물

시약·촉매·용매 3

HCID 142844-(Dimethylamino)pyridine촉매HCID 962Water용매HCID 6344Dichloromethane용매3회

실험 절차

In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), a solution of 5-phenyl-oxazole-4-carboxylic acid (47 mg, 0.25 mmol) in CH2Cl2 (1.5 mL) was treated at rt with HOBt (40 mg, 0.30 mmol), EDC (119 mg, 0.62 mmol), DMAP (8 mg, 0.06 mmol) and the resulting mixture was stirred at rt for 30 min. 2-{2-[1-(tert-Butyl-dimethyl-silanyloxy)-ethyl]-oxazol-5-ylmethyl}-2H-[1,2,3]triazol-4-ylamine (80 mg, 0.25 mmol) in CH2Cl2 (1.0 mL) was then added and the resulting mixture was stirred at rt for 72 h. CH2Cl2 (20 mL) followed by water (15 mL) were added and the aqueous phase was extracted with CH2Cl2. The combined organic phases were washed with water, brine, dried over MgSO4, filtered, and the solvent removed under reduced pressure to give the title compound as a yellow oil. LC-MS-conditions 02: tR=1.17 min, [M+H]+=495.54.

후처리

  1. stirringthe resulting mixture was stirred at rt for 72 h
  2. additionwere added
  3. extractionthe aqueous phase was extracted with CH2Cl2
  4. washThe combined organic phases were washed with water, brine
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. customthe solvent removed under reduced pressure

출처 및 근거

ORD 기록
ord-d09c9e4e9e4d497480759f445fc478c3
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08536209B2

연결된 노트

불러오는 중…