HCID 71000688, 화합물 → HCID 69081573, 화합물

HRID 1023455노트

반응식

HRID 1023455 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]#[C:9][C:10]2[CH:15]=[CH:14][N:13]=[C:12]([NH:16][C:17]([NH2:19])=[O:18])[CH:11]=2)=[C:4]([CH3:20])[CH:3]=1.[H][H]>CO.C(Cl)Cl.[Pd]>[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH2:9][C:10]2[CH:15]=[CH:14][N:13]=[C:12]([NH:16][C:17]([NH2:19])=[O:18])[CH:11]=2)=[C:4]([CH3:20])[CH:3]=1

참가 물질

6

반응물 2

HCID 71000688HCID 71000688, 화합물HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 69081573HCID 69081573, 화합물수율 70.8%

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 887Methanol용매2회HCID 6344Dichloromethane용매

실험 절차

[4-(4-Fluoro-2-methyl-phenylethynyl)-pyridin-2-yl]-urea (25 mg, 0.093 mmol) is dissolved in methanol (1.0 mL) and DCM (1.0 mL). Then 5% palladium on carbon (20 mg, 0.0090 mmol) is added. The reaction is stirred for 16 hrs under the hydrogen atmosphere. The palladium on carbon is filtered and the filtrate is concentrated to give the crude product. Methanol (1 mL) is added into the crude and a white solid is formed. The solid is filtered, rinsed with more methanol and dried to give 18 mg of the titled product.

후처리

  1. filtrationThe palladium on carbon is filtered
  2. concentrationthe filtrate is concentrated
  3. customto give the crude product
  4. customa white solid is formed
  5. filtrationThe solid is filtered
  6. washrinsed with more methanol
  7. customdried

출처 및 근거

ORD 기록
ord-487953f7d2e64fafac075067ece294c6
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08722709B2

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