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Methanol → HCID 18925028, 화합물

HRID 1869104
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HRID 1869104 반응식
Cl.[Cl:2][C:3]1[CH:12]=[C:11]2[C:6]([C:7]([NH:13][C:14]3[CH:19]=[CH:18][CH:17]=[C:16]([C:20]#[CH:21])[CH:15]=3)=[N:8][CH:9]=[N:10]2)=[CH:5][C:4]=1[N+:22]([O-])=O.S(S([O-])=O)([O-])=O.[Na+].[Na+].CO>C(O)=O>[ClH:2].[NH2:22][C:4]1[CH:5]=[C:6]2[C:11](=[CH:12][C:3]=1[Cl:2])[N:10]=[CH:9][N:8]=[C:7]2[NH:13][C:14]1[CH:19]=[CH:18][CH:17]=[C:16]([C:20]#[CH:21])[CH:15]=1
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참가 물질

5

반응물 3

HCID 887MethanolHCID 24489Sodium DithioniteHCID 18925030HCID 18925030, 화합물

생성물 1

HCID 18925028HCID 18925028, 화합물

시약·촉매·용매 1

HCID 284Formic Acid용매

실험 절차

(7-Chloro-6-nitro-quinazolin-4-yl)-(3-ethynyl-phenyl)-amine hydrochloride (166 mg, 0.295 mmol) and sodium dithionite (207 mg, 1.19 mmol) were stirred in 1.5 mL of formic acid for 4 hours at room temperature. 45 mL of methanol were added to the reaction mixture which was set aside for 16 hours at room temperature. The precipitate thus obtained was filtered, triturated with 3% sodium bicarbonate for 0.5 hours and refiltered. The solid was dissolved in 20 mL of 1N HCl in methanol and precipitated with 200 mL of ethyl ether. This was filtered and dried in vacuo at 70° C. to afford the title product, 72 mg (83%); mp 260°-265° C.

후처리

  1. customThe precipitate thus obtained
  2. filtrationwas filtered
  3. customtriturated with 3% sodium bicarbonate for 0.5 hours
  4. dissolutionThe solid was dissolved in 20 mL of 1N HCl in methanol
  5. customprecipitated with 200 mL of ethyl ether
  6. filtrationThis was filtered
  7. customdried in vacuo at 70° C.

출처 및 근거

ORD 기록
ord-64d8424690904939b7f8496c2c9b39de
출처 데이터셋
uspto-grants-2009_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
USRE041065E1

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