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 494131ノート

反応式

HRID 494131 の反応式
[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

参加物

3

反応物 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

生成物 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

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-bb1fc5961f52474da6ddb0b1097b1962
出典データセット
uspto-grants-2009_05
特許番号
US07538112B2

反応ノート

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