Choline, hydroxide → HCID 178492086、化合物

HRID 323641

反応式

HRID 323641 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[C:6](=[O:27])[C:7]3[C:15](=[O:16])[N:14]([C:17]4[CH:22]=[CH:21][C:20]([O:23][CH3:24])=[CH:19][C:18]=4[CH3:25])[N:13]=[C:12]([OH:26])[C:8]=3[NH:9][C:10]=2[CH:11]=1.[OH-].[OH:29][CH2:30][CH2:31][N+:32]([CH3:35])([CH3:34])[CH3:33]>CO>[OH:29][CH2:30][CH2:31][N+:32]([CH3:35])([CH3:34])[CH3:33].[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[C:6](=[O:27])[C:7]3[C:15](=[O:16])[N:14]([C:17]4[CH:22]=[CH:21][C:20]([O:23][CH3:24])=[CH:19][C:18]=4[CH3:25])[N:13]=[C:12]([OH:26])[C:8]=3[NH:9][C:10]=2[CH:11]=1

参加物

4

反応物 2

HCID 31255Choline, hydroxideHCID 178492085HCID 178492085、化合物

生成物 1

HCID 178492086HCID 178492086、化合物収率 81%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a stirred suspension of 7-chloro-4-hydroxy-2-(4-methoxy-2-methylphenyl)-1,2,5,10-tetrahydropyridazino[4,5-b]quinoline-1,10-dione (400 mg, 1.03 mM) in methanol (4 mL) was added choline hydroxide (45% by weight in methanol, 295.6 μL, 1.03 mM). After brief sonication, all solids dissolved and the resulting solution was filtered through a Gelman Glass Acrodisc filter (0.45 μm) along with an additional quantity of methanol (8 mL). The filtrate was concentrated to dryness and the residual oil was stirred with isopropanol (15 mL) and ethanol (8 mL) whereupon crystallization occurred. The solids were collected and dried under vacuum at 100° C. overnight to give the title compound (411 mg, 81 %) as a yellow solid, mp 229-230° C.

後処理

  1. customAfter brief sonication
  2. dissolutionall solids dissolved
  3. filtrationthe resulting solution was filtered through a Gelman Glass Acrodisc
  4. filtrationfilter (0.45 μm) along with an additional quantity of methanol (8 mL)
  5. concentrationThe filtrate was concentrated to dryness
  6. customThe solids were collected
  7. customdried under vacuum at 100° C. overnight

出典と根拠

ORDレコード
ord-be2697b12ea94cd685131646bfe8815a
出典データセット
uspto-grants-2001_04
特許番号
US06214826B1

関連ノート

読み込み中…