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Water → 4-amino-5-chloro-2-methoxy-N-[(2S,4S)-2-hydroxymethyl-4-pyrrolidinyl]benzamide monohydrochloride

HRID 1723905
ノート
印刷プレビュー

反応式

HRID 1723905 の反応式
C([NH:4][C:5]1[C:23]([Cl:24])=[CH:22][C:8]([C:9]([NH:11][C@@H:12]2[CH2:16][N:15](C(=O)C)[C@H:14]([CH2:20][OH:21])[CH2:13]2)=[O:10])=[C:7]([O:25][CH3:26])[CH:6]=1)(=O)C.[OH-].[Na+].O>C(O)C>[ClH:24].[NH2:4][C:5]1[C:23]([Cl:24])=[CH:22][C:8]([C:9]([NH:11][C@@H:12]2[CH2:16][NH:15][C@H:14]([CH2:20][OH:21])[CH2:13]2)=[O:10])=[C:7]([O:25][CH3:26])[CH:6]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 117406984-acetylamino-5-chloro-2-methoxy-N-[(2S,4S)-1-acetyl-2-hydroxymethyl-4-pyrrolidinyl]benzamide

生成物 1

HCID 690168684-amino-5-chloro-2-methoxy-N-[(2S,4S)-2-hydroxymethyl-4-pyrrolidinyl]benzamide monohydrochloride収率 107%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

11.74 g of 4-acetylamino-5-chloro-2-methoxy-N-[(2S,4S)-1-acetyl-2-hydroxymethyl-4-pyrrolidinyl]benzamide was dissolved in ethyl alcohol (60 ml), and sodium hydroxide (2.7 g) was added thereto. The mixture was heated at reflux for 8.5 hours. After addition of water (20 ml), the mixture was stirred at room temperature for 1 hour to filter insolubles off, and washed sufficiently with water (50 ml). The filtrate was concentrated under reduced pressure, n-butyl alcohol (50 ml) and a saturated brine solution (20 ml) were added to the resulting residue, and the layers were separated, followed by re-extraction with n-butyl alcohol (30 ml). The extract was concentrated under reduced pressure, methyl alcohol (50 ml) was added to the residue to dissolve it, and 18% (w/w) hydrochloric acid-containing methyl alcohol (6.5 g) was gradually added to adjust to a pH 6. After ice-cooling, precipitated crystals were filtered, and washed with a small amount of methyl alcohol. The resulting crystals were recrystallized from ethyl alcohol to obtain 5.5 g of the objective 4-amino-5-chloro-2-methoxy-N-[(2S,4S)-2-hydroxymethyl-4-pyrrolidinyl]benzamide monohydrochloride. mp 219-222° C., [α]D20: +4.20 (c=1.00, EtOH)

後処理

  1. temperatureThe mixture was heated
  2. temperatureat reflux for 8.5 hours
  3. filtrationto filter insolubles off, and
  4. washwashed sufficiently with water (50 ml)
  5. concentrationThe filtrate was concentrated under reduced pressure, n-butyl alcohol (50 ml)
  6. additiona saturated brine solution (20 ml) were added to the resulting residue
  7. customthe layers were separated
  8. extractionfollowed by re-extraction with n-butyl alcohol (30 ml)
  9. concentrationThe extract was concentrated under reduced pressure, methyl alcohol (50 ml)
  10. additionwas added to the residue
  11. dissolutionto dissolve it, and 18% (w/w) hydrochloric acid-
  12. additioncontaining methyl alcohol (6.5 g)
  13. additionwas gradually added
  14. temperatureAfter ice-cooling
  15. customprecipitated crystals
  16. filtrationwere filtered
  17. washwashed with a small amount of methyl alcohol
  18. customThe resulting crystals were recrystallized from ethyl alcohol

出典と根拠

ORDレコード
ord-215f385f87524e668736f5d8c4bf1521
出典データセット
uspto-grants-2009_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07485665B2

反応ノート

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