Hydrochloric Acid → HCID 69315002、化合物

HRID 1391713ノート

反応式

HRID 1391713 の反応式
[Li+].[OH-].O.[C:4]([NH:7][C@:8]1([CH:22]([CH2:24][CH3:25])[CH3:23])[CH2:12][CH2:11][N:10]([C@@H:13]([CH2:18][CH:19]=[CH2:20])[C:14]([O:16]C)=[O:15])[C:9]1=[O:21])(=[O:6])[CH3:5].Cl>C1COCC1>[C:4]([NH:7][C@:8]1([CH:22]([CH2:24][CH3:25])[CH3:23])[CH2:12][CH2:11][N:10]([C@@H:13]([CH2:18][CH:19]=[CH2:20])[C:14]([OH:16])=[O:15])[C:9]1=[O:21])(=[O:6])[CH3:5]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 168937Lithium hydroxide, monohydrateHCID 69316592(s)-Methyl 2-((s)-3-acetamido-3-sec-butyl-2-oxopyrrolidin-1-yl)pent-4-enoate

生成物 1

HCID 69315002HCID 69315002、化合物収率 88.2%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Step L (7): A solution of LiOH/H2O (2M, 28 mg in 0.50 mL) was added to the diastereomer B, (S)-methyl 2-((S)-3-acetamido-3-sec-butyl-2-oxopyrrolidin-1-yl)pent-4-enoate (122 mg, 0.39 mmol) from Step L (6) in THF (1.0 mL) at RT. The reaction was stirred for 3 days. The mixture was poured into 1N HCl and the aqueous layer was extracted with EtOAC. The combined organic layers were washed with brine, dried over NaSO4 and concentrated in vacuo to give 102 mg of the title compound as white solid. LC-MS (M+H)+=297.01.

後処理

  1. extractionthe aqueous layer was extracted with EtOAC
  2. washThe combined organic layers were washed with brine
  3. dry with materialdried over NaSO4
  4. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-99cbc239ed154870975f576a4d3ff0b8
出典データセット
uspto-grants-2008_03
特許番号
US07338974B2

反応ノート

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