Thionyl Chloride → 2-(4-Fluorobenzyl)-10-methoxy-4-(1-chloroethyl)-8-methyl-7,8-dihydropyrazino[1',2':1,5]pyrrolo[2,3-d]pyridazine-1,9(2H,6H)-dione

HRID 494131노트

반응식

HRID 494131 반응식
[F:1][C:2]1[CH:29]=[CH:28][C:5]([CH2:6][N:7]2[C:12](=[O:13])[C:11]3[C:14]([O:23][CH3:24])=[C:15]4[C:20](=[O:21])[N:19]([CH3:22])[CH2:18][CH2:17][N:16]4[C:10]=3[C:9]([CH:25](O)[CH3:26])=[N:8]2)=[CH:4][CH:3]=1.S(Cl)([Cl:32])=O>>[F:1][C:2]1[CH:29]=[CH:28][C:5]([CH2:6][N:7]2[C:12](=[O:13])[C:11]3[C:14]([O:23][CH3:24])=[C:15]4[C:20](=[O:21])[N:19]([CH3:22])[CH2:18][CH2:17][N:16]4[C:10]=3[C:9]([CH:25]([Cl:32])[CH3:26])=[N:8]2)=[CH:4][CH:3]=1

참가 물질

3

반응물 2

HCID 24386Thionyl ChlorideHCID 688652402-(4-Fluorobenzyl)-10-methoxy-4-(1-hydroxyethyl)-8-methyl-7,8-dihydropyrazino[1',2':1,5]pyrrolo[2,3-d]pyridazine-1,9(2H,6H)-dione

생성물 1

HCID 688663392-(4-Fluorobenzyl)-10-methoxy-4-(1-chloroethyl)-8-methyl-7,8-dihydropyrazino[1',2':1,5]pyrrolo[2,3-d]pyridazine-1,9(2H,6H)-dione

실험 절차

A solution of 2-(4-fluorobenzyl)-10-methoxy-4-(1-hydroxyethyl)-8-methyl-7,8-dihydropyrazino[1′,2′:1,5]pyrrolo[2,3-d]pyridazine-1,9(2H,6H)-dione (0.12 g, 0.30 mmol) in thionyl chloride (3.3 mL) was stirred at room temperature for 3 hours. The reaction mixture was concentrated under vacuum. The residue was concentrated from a solution in benzene under vacuum and triturated with diethyl ether. The solid precipitated was filtered and vacuum dried to provide the title compound.

후처리

  1. concentrationThe reaction mixture was concentrated under vacuum
  2. concentrationThe residue was concentrated from a solution in benzene under vacuum
  3. customtriturated with diethyl ether
  4. customThe solid precipitated
  5. filtrationwas filtered
  6. customvacuum dried

출처 및 근거

ORD 기록
ord-bb1fc5961f52474da6ddb0b1097b1962
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07538112B2

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