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Hydrochloric Acid → HCID 178485275、化合物

HRID 922727
ノート
印刷プレビュー

反応式

HRID 922727 の反応式
[Cl-].[Ca+2].[Cl-].[BH4-].[Na+].[OH:6][C@@:7]([C:29]1[CH:38]=[CH:37][C:36]2[C:31](=[CH:32][CH:33]=[C:34]([C:39]([NH:41][CH3:42])=[O:40])[CH:35]=2)[CH:30]=1)([C:14]1[N:15]=[CH:16][N:17](S(C2C=CC(C)=CC=2)(=O)=O)[CH:18]=1)[CH2:8][C:9](OCC)=[O:10].Cl.[OH-].[Na+]>C(O)C.O1CCCC1.O.C(OCC)(=O)C>[OH:6][C@@:7]([C:29]1[CH:30]=[C:31]2[C:36](=[CH:37][CH:38]=1)[CH:35]=[C:34]([C:39]([NH:41][CH3:42])=[O:40])[CH:33]=[CH:32]2)([C:14]1[N:15]=[CH:16][NH:17][CH:18]=1)[CH2:8][CH2:9][OH:10]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

10

反応物 5

HCID 313Hydrochloric Acid3 回HCID 14798Sodium Hydroxide3 回HCID 4311764Sodium borohydrideHCID 5284359Calcium ChlorideHCID 86715405ethyl (3S)-3-hydroxy-3-{6-[(methylamino)carbonyl]-2-naphthyl}-3-(1-tosyl-1H-imidazol-4-yl)propanoate

生成物 1

HCID 178485275HCID 178485275、化合物
収率 125%

試薬・触媒・溶媒 4

HCID 702Ethanol溶媒3 回HCID 962Water溶媒3 回HCID 8028Tetrahydrofuran溶媒2 回HCID 8857Ethyl Acetate溶媒

反応条件

温度
-10 °C

実験手順

To a solution of anhydrous calcium chloride (1.86 g, 16.3 mmol) in ethanol (32 mL) were added sodium borohydride (1.27 g, 33.6 mmol) and ethanol (5 mL) at −10° C., and the mixture was stirred at −10° C. for 30 min. To the reaction mixture was added dropwise a solution of ethyl (3S)-3-hydroxy-3-{6-[(methylamino)carbonyl]-2-naphthyl}-3-(1-tosyl-1H-imidazol-4-yl)propanoate (2.5 g, 5.6 mmol) in tetrahydrofuran (73 mL)/ethanol (10 mL), and tetrahydrofuran (5 mL) at −10° C. The obtained reaction mixture was stirred at 7° C. for 21 hr, and to the obtained reaction mixture were added dropwise water (100 mL), 1 mol/L hydrochloric acid (40 mL) and ethyl acetate (200 mL) at 10° C. or below, and the mixture was stirred. To the separated organic layer was added 0.2 mol/L hydrochloric acid (14 mL) at 5° C., and the mixture was stirred. The reaction mixture was adjusted to pH 7.5 with 0.5 mol/L aqueous sodium hydroxide solution at 5° C. To the separated organic layer was added again 0.2 mol/L hydrochloric acid (14 mL) at 5° C., and the mixture was stirred. The reaction mixture was adjusted to pH 7.5 with 0.5 mol/L aqueous sodium hydroxide solution at 5° C. To the separated organic layer was added water (10 mL), and the mixture was adjusted to pH 9.5 with 0.5 mol/L aqueous sodium hydroxide solution. To the separated organic layer was added water (120 mL), and the mixture was heated to 60° C., and stirred for 3 hr. The separated organic layer was concentrated at 60° C. under reduced pressure to give 6-[(1S)-1,3-dihydroxy-1-(1H-imidazol-4-yl)propyl]-N-methyl-2-naphthamide (2.3 g, 7.0 mmol).

後処理

  1. customThe obtained reaction mixture
  2. stirringwas stirred at 7° C. for 21 hr
  3. customto the obtained reaction mixture
  4. stirringthe mixture was stirred
  5. stirringthe mixture was stirred
  6. stirringthe mixture was stirred
  7. temperaturethe mixture was heated to 60° C.
  8. stirringstirred for 3 hr
  9. concentrationThe separated organic layer was concentrated at 60° C. under reduced pressure

出典と根拠

ORDレコード
ord-9b7c8bae98e54e43b5007e0a0eeb3ec6
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09278938B2

反応ノート

読み込み中…

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