Water → HCID 178418468、化合物

HRID 1695

反応式

HRID 1695 の反応式
[C:1]([NH:8][C@H:9]1[CH2:14][CH2:13][C@@H:12]([C:15]([O:17][C:18]2[CH:27]=[CH:26][C:21]([C:22]([O:24]C)=[O:23])=[C:20]([O:28][CH3:29])[CH:19]=2)=[O:16])[CH2:11][CH2:10]1)([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].O.O[Li].O>C1COCC1>[C:1]([NH:8][C@H:9]1[CH2:14][CH2:13][C@@H:12]([C:15]([O:17][C:18]2[CH:27]=[CH:26][C:21]([C:22]([OH:24])=[O:23])=[C:20]([O:28][CH3:29])[CH:19]=2)=[O:16])[CH2:11][CH2:10]1)([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2]

参加物

5

反応物 3

HCID 962WaterHCID 168937Lithium hydroxide, monohydrateHCID 178418455HCID 178418455、化合物

生成物 1

HCID 178418468HCID 178418468、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
45 °C

実験手順

To a stirred solution of methyl 4-[N-Boc-cis-1-amino-4-cyclohexanoyloxy]-2-methoxybenzoate (220 mg, 0.52 mmol) in THF:H2O (5 mL: 1 mL) was added LiOH.H2O (67.6 mg, 1.59 mmol). The reaction was heated to 45° C. over 12 h and then cooled to ambient temperature. The solvent was removed under reduced pressure. The crude solid passed through a plug of silca gel packed in 50:50 MeOH:CH2Cl2 and eluted with same. The solvent was removed under reduced pressure to afford 4-[N-Boc-cis-1-amino-4-cyclohexanoyloxy]-2-methoxybenzoic acid as a white solid.

後処理

  1. temperaturecooled to ambient temperature
  2. customThe solvent was removed under reduced pressure
  3. washCH2Cl2 and eluted with same
  4. customThe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-c883c9ea34ed4863b03fce02c544723e
出典データセット
uspto-grants-1998_03
特許番号
US05726172

関連ノート

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