Choline, hydroxide → HCID 178492086, 화합물

HRID 1977224

반응식

HRID 1977224 반응식
[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

참가 물질

4

반응물 2

HCID 31255Choline, hydroxideHCID 178492085HCID 178492085, 화합물

생성물 1

HCID 178492086HCID 178492086, 화합물수율 81%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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 uL, 1.03 mM). After brief sonication, all solids dissolved and the resulting solution was filtered through a Gelman Glass Acrodisc filter (0.45 um) 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.

후처리

  1. customAfter brief sonication
  2. dissolutionall solids dissolved
  3. filtrationthe resulting solution was filtered through a Gelman Glass Acrodisc
  4. filtrationfilter (0.45 um) 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

출처 및 근거

ORD 기록
ord-965d3350f4e84356986f7cd2367d4a99
출처 데이터셋
uspto-grants-2001_05
특허 번호
US06232313B1

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