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HCID 59389278、化合物 → HCID 59389404、化合物

HRID 2357921
ノート
印刷プレビュー

反応式

HRID 2357921 の反応式
C[Mg]Br.O1CCC[CH2:5]1.[CH:9]([C:11]1[CH:29]=[C:14]2[C:15]([C:21]3[CH:22]([CH3:28])[CH2:23][C:24](=[O:27])[NH:25][N:26]=3)=[CH:16][CH:17]=[C:18]([O:19][CH3:20])[N:13]2[N:12]=1)=[O:10]>C1COCC1>[OH:10][CH:9]([C:11]1[CH:29]=[C:14]2[C:15]([C:21]3[CH:22]([CH3:28])[CH2:23][C:24](=[O:27])[NH:25][N:26]=3)=[CH:16][CH:17]=[C:18]([O:19][CH3:20])[N:13]2[N:12]=1)[CH3:5]
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 59389278HCID 59389278、化合物HCID 178420675HCID 178420675、化合物

生成物 1

HCID 59389404HCID 59389404、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A 0.90 mol/L methyl magnesium bromide-tetrahydrofuran solution (0.878 mL) was added dropwise to a solution of the compound of Example 237 (90.6 mg) in THF (15 mL) at −78° C. in an argon atmosphere. The mixture was allowed to gradually warm to room temperature. The reaction was quenched by adding a saturated aqueous solution of ammonium chloride and the mixture was extracted with THF (100 mL). The extract was washed with water and saturated brine and dried over anhydrous sodium sulfate. The dried extract was concentrated and purified by recrystallization (methanol-ethyl acetate-hexane) to afford the title compound as a pale yellow powder (38.0 mg).

後処理

  1. customThe reaction was quenched
  2. additionby adding a saturated aqueous solution of ammonium chloride
  3. extractionthe mixture was extracted with THF (100 mL)
  4. washThe extract was washed with water and saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. extractionThe dried extract
  7. concentrationwas concentrated
  8. custompurified by recrystallization (methanol-ethyl acetate-hexane)

出典と根拠

ORDレコード
ord-78e704d923f24aaeb25d31892cfddfe1
出典データセット
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07763617B2

反応ノート

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