Hydrochloric Acid → HCID 178487512、化合物

HRID 651599

反応式

HRID 651599 の反応式
Cl[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([CH2:12][N:13]3[CH2:17][CH2:16][C@H:15]([NH:18][S:19]([C:22]4[CH:31]=[CH:30][C:29]5[C:24](=[CH:25][C:26]([O:32][CH3:33])=[CH:27][CH:28]=5)[CH:23]=4)(=[O:21])=[O:20])[C:14]3=[O:34])[CH:10]=2)[CH:5]=[CH:4][N:3]=1.[OH-:35].[Na+].Cl>O1CCOCC1>[OH:35][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([CH2:12][N:13]3[CH2:17][CH2:16][CH:15]([NH:18][S:19]([C:22]4[CH:31]=[CH:30][C:29]5[C:24](=[CH:25][C:26]([O:32][CH3:33])=[CH:27][CH:28]=5)[CH:23]=4)(=[O:21])=[O:20])[C:14]3=[O:34])[CH:10]=2)[CH:5]=[CH:4][N:3]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 155458317-Methoxy-naphthalene-2-sulfonic acid[1-(1-chloro-isoquinolin-7-ylmethyl)-2-oxopyrrolidin-3-(s)-yl]-amide

生成物 1

HCID 178487512HCID 178487512、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

7-Methoxynaphthalene-2-sulfonic acid [1-(1-chloro-isoquinolin-7-ylmethyl)-2-oxopyrrolidin-3-(S)-yl]amide (0.07 g, 0.14 mmol), prepared as described in EXAMPLE 1, Part K, is treated with dioxane (1 mL) and 10% aq. NaOH (3 mL) and heated to reflux for 48 hours. The reaction was cooled, acidified with 1 N HCl and extracted with CH2Cl2. The organic layer is separated, dried and concentrated. The residue is purified by column chromatography eluting with 2.5% MeOH/CH2Cl2. The product fractions are collected, concentrated and precipitated with dilute HCl/ether to yield the title compound (0.041 g, 0.086 mmol).

後処理

  1. temperatureheated
  2. temperatureto reflux for 48 hours
  3. temperatureThe reaction was cooled
  4. extractionextracted with CH2Cl2
  5. customThe organic layer is separated
  6. customdried
  7. concentrationconcentrated
  8. customThe residue is purified by column chromatography
  9. washeluting with 2.5% MeOH/CH2Cl2
  10. customThe product fractions are collected
  11. concentrationconcentrated
  12. customprecipitated with dilute HCl/ether

出典と根拠

ORDレコード
ord-909cad4e41604bd6ab20d4d1fb720db6
出典データセット
uspto-grants-2001_08
特許番号
US06281227B1

関連ノート

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