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Lithium Hydroxide → HCID 118157541、化合物

HRID 1779198
ノート
印刷プレビュー

反応式

HRID 1779198 の反応式
C([O:4][CH2:5][CH2:6][C@:7]([OH:49])([C@@H:11]([C:29](=[O:48])[NH:30][C@H:31]([C:44]([O:46]C)=[O:45])[CH2:32][C:33]1[CH:38]=[CH:37][C:36]([O:39][CH2:40][C:41]#[C:42][CH3:43])=[CH:35][CH:34]=1)/[CH:12]=[CH:13]/[CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][C:20](=[O:28])[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH3:27])[C:8]([OH:10])=[O:9])(=O)C.[Li+].[OH-]>CO>[CH2:40]([O:39][C:36]1[CH:37]=[CH:38][C:33]([CH2:32][C@H:31]([NH:30][C:29]([C@@H:11](/[CH:12]=[CH:13]/[CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][C:20](=[O:28])[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH3:27])[C@@:7]([OH:49])([CH2:6][CH2:5][OH:4])[C:8]([OH:10])=[O:9])=[O:48])[C:44]([OH:46])=[O:45])=[CH:34][CH:35]=1)[C:41]#[C:42][CH3:43]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 3939Lithium HydroxideHCID 90060133HCID 90060133、化合物

生成物 1

HCID 118157541HCID 118157541、化合物収率 18.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

No. 5214354, (E)-(2S,3S)-2-(2-acetoxy-ethyl)-3-[(S)-2-(4-but-2-ynyloxy-phenyl)-1-methoxycarbonyl-ethylcarbamoyl]-2-hydroxy-12-oxo-nonadec-4-enoic acid (120 mg, 0.175 mmol) was dissolved in methanol (10 mL), and an aqueous solution (1 mL) of 2 M LiOH was added, and the mixture was stirred at room temperature. After confirming the consumption of the starting materials by LCMS, methanol was distilled off under reduced pressure. To the residue was added 1 M hydrochloric acid, and the mixture was extracted with ethyl acetate. The organic layer was washed with a saturated brine and then dried over anhydrous sodium sulfate. The filtrate was concentrated under reduced pressure. The resulting residue was purified by preparative HPLC and freeze-dried to obtain the title compound (20 mg, 18% yield, white powder).

後処理

  1. customthe consumption of the starting materials by LCMS, methanol
  2. distillationwas distilled off under reduced pressure
  3. additionTo the residue was added 1 M hydrochloric acid
  4. extractionthe mixture was extracted with ethyl acetate
  5. washThe organic layer was washed with a saturated brine
  6. dry with materialdried over anhydrous sodium sulfate
  7. concentrationThe filtrate was concentrated under reduced pressure
  8. customThe resulting residue was purified by preparative HPLC
  9. customfreeze-dried

出典と根拠

ORDレコード
ord-24d1e5860b0f45aca002d71ce3041ad4
出典データセット
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09266853B2

反応ノート

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