Hydrochloric Acid → HCID 178463212、化合物

HRID 1469163ノート

反応式

HRID 1469163 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([N:13]([C@H:16]2[CH2:21][CH2:20][C@H:19]([N:22](C(OC(C)(C)C)=O)[CH3:23])[CH2:18][CH2:17]2)[CH2:14][CH3:15])[C:5]([CH3:12])=[C:6]([CH:11]=1)[C:7]([O:9][CH3:10])=[O:8].Cl>CO>[Br:1][C:2]1[CH:3]=[C:4]([N:13]([CH2:14][CH3:15])[C@H:16]2[CH2:21][CH2:20][C@H:19]([NH:22][CH3:23])[CH2:18][CH2:17]2)[C:5]([CH3:12])=[C:6]([CH:11]=1)[C:7]([O:9][CH3:10])=[O:8]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 178463214HCID 178463214、化合物

生成物 1

HCID 178463212HCID 178463212、化合物収率 104.8%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a stirred solution of methyl 5-bromo-3-(((trans)-4-((tert-butoxycarbonyl)(methyl)amino)cyclohexyl)(ethyl)amino)-2-methylbenzoate (30 g, 62.24 mmol) in methanol (100 mL) at 0° C., methanolic HCl (500 mL) was added and reaction was stirred for 2 h at room temperature. After completion, reaction was concentrated to dryness. The residue was basified with Na2CO3 (aq.) to pH 8 and aqueous layer was extracted with 10% methanol in DCM (200 mL×3). Combined organic layers were dried over Na2SO4 and solvent removed under reduced pressure to afford the title compound as colorless oil (25 g, crude). The isolated compound was used in the next step without further purification.

後処理

  1. customreaction
  2. customAfter completion, reaction
  3. concentrationwas concentrated to dryness
  4. extractionwas extracted with 10% methanol in DCM (200 mL×3)
  5. dry with materialCombined organic layers were dried over Na2SO4 and solvent
  6. customremoved under reduced pressure

出典と根拠

ORDレコード
ord-6a60ed99747a42f495146ceff710117a
出典データセット
uspto-grants-2015_04
特許番号
US09006242B2

反応ノート

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