Methanol → HCID 49872352, 화합물

HRID 80159

반응식

HRID 80159 반응식
[S:1]1[C:5]2[CH:6]=[C:7]([N:10]3[CH2:14][CH2:13][N:12]([C:15]4[CH:16]=[N:17][CH:18]=[CH:19][C:20]=4Cl)[C:11]3=[O:22])[CH:8]=[CH:9][C:4]=2[N:3]=[CH:2]1.[CH3:23][O-:24].[Na+].CO>O1CCOCC1.C(Cl)(Cl)Cl>[S:1]1[C:5]2[CH:6]=[C:7]([N:10]3[CH2:14][CH2:13][N:12]([C:15]4[CH:16]=[N:17][CH:18]=[CH:19][C:20]=4[O:24][CH3:23])[C:11]3=[O:22])[CH:8]=[CH:9][C:4]=2[N:3]=[CH:2]1

참가 물질

6

반응물 3

HCID 887MethanolHCID 10942334Sodium MethoxideHCID 596362211-Benzothiazol-6-yl-3-(4-chloro-pyridin-3-yl)-imidazolidin-2-one

생성물 1

HCID 49872352HCID 49872352, 화합물수율 32.4%

시약·촉매·용매 2

HCID 6212Chloroform용매HCID 312751,4-Dioxane용매

실험 절차

1-Benzothiazol-6-yl-3-(4-chloro-pyridin-3-yl)-imidazolidin-2-one (84A: 50 mg, 0.1515 mmol) was added dropwise to a solution of sodium methoxide (0.122 g, 2.259 mmol) in 1,4-dioxane (15 mL) over a period of 5 minutes. The resulting mixture was refluxed for 10 hours. The reaction was monitored by TLC (10% MeOH in CHCl3). The reaction mixture was partitioned between ice water and ethylacetate. The organic layer was dried over Na2SO4 and concentrated. Purification by preparative HPLC afforded 16 mg of the product (31.66% yield).

후처리

  1. temperatureThe resulting mixture was refluxed for 10 hours
  2. customThe reaction mixture was partitioned between ice water and ethylacetate
  3. dry with materialThe organic layer was dried over Na2SO4
  4. concentrationconcentrated
  5. customPurification by preparative HPLC

출처 및 근거

ORD 기록
ord-d12f0dd3f7b44cb18ce6da01dfe0f625
출처 데이터셋
uspto-grants-2014_09
특허 번호
USRE045173E1

연결된 노트

불러오는 중…