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Sodium Hydroxide → 2-[1-[1-(4-Methoxy-2-methylphenyl)-6-methyl-2,3-dihydropyrrolo[2,3-b]pyridin-4-yl]pyrazol-3-yl]-1,2,5-thiadiazolidine 1,1-dioxide

HRID 32802
ノート
印刷プレビュー

反応式

HRID 32802 の反応式
[CH3:1][C:2]1[N:7]=[C:6]2[N:8]([C:11]3[CH:16]=[CH:15][C:14]([O:17][CH3:18])=[CH:13][C:12]=3[CH3:19])[CH2:9][CH2:10][C:5]2=[C:4]([N:20]2[CH:24]=[CH:23][C:22]([N:25]3[S:29](=[O:31])(=[O:30])[N:28](C(OC)=O)[CH2:27][CH2:26]3)=[N:21]2)[CH:3]=1.[OH-].[Na+].C([O-])(O)=O.[Na+]>CO.C(Cl)Cl>[O:31]=[S:29]1(=[O:30])[NH:28][CH2:27][CH2:26][N:25]1[C:22]1[CH:23]=[CH:24][N:20]([C:4]2[CH:3]=[C:2]([CH3:1])[N:7]=[C:6]3[N:8]([C:11]4[CH:16]=[CH:15][C:14]([O:17][CH3:18])=[CH:13][C:12]=4[CH3:19])[CH2:9][CH2:10][C:5]=23)[N:21]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 14798Sodium HydroxideHCID 516892Sodium BicarbonateHCID 11306561HCID 11306561、化合物

生成物 1

HCID 112476722-[1-[1-(4-Methoxy-2-methylphenyl)-6-methyl-2,3-dihydropyrrolo[2,3-b]pyridin-4-yl]pyrazol-3-yl]-1,2,5-thiadiazolidine 1,1-dioxide収率 100.9%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒
HCID 6344
Dichloromethane
溶媒
2 回

実験手順

To a solution of example 5-1 (7.2 mg, 0.0144 mmol) in anh. MeOH (1 mL) and anh. CH2Cl2 (2 mL), at r.t., under N2, was added 25% NaOH (40 μL). The reaction mixture was stirred at r.t. for 30 min. It was then poured into sat.aq. NaHCO3 and CH2Cl2 was added. The phases were separated and the aqueous layer was further extracted with CH2Cl2 (2×10 mL). The combined organic extracts were dried over anh. Na2SO4, the solids were filtered and the solvent evaporated to give the title compound (6.4 mg, quantitative yield) as a white solid.

後処理

  1. additionIt was then poured into sat.aq
  2. customThe phases were separated
  3. extractionthe aqueous layer was further extracted with CH2Cl2 (2×10 mL)
  4. dry with materialThe combined organic extracts were dried over anh. Na2SO4
  5. filtrationthe solids were filtered
  6. customthe solvent evaporated

出典と根拠

ORDレコード
ord-e8af4723cfc24a4badd9fd577fba28a5
出典データセット
uspto-grants-2008_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07427630B2

反応ノート

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