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Formaldehyde → HCID 11596500、化合物

HRID 1516146
ノート
印刷プレビュー

反応式

HRID 1516146 の反応式
[CH3:1][O:2][C:3](=[O:28])/[C:4](/[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[CH2:14][O:15][C:16]1[CH:21]=[CH:20][C:19]([NH:22][CH2:23][CH:24]([CH3:26])[CH3:25])=[CH:18][C:17]=1[F:27])=[CH:5]/[O:6][CH3:7].[BH-](OC(C)=O)(OC(C)=O)O[C:31](C)=O.[Na+].C=O.C(=O)(O)[O-].[Na+]>C(Cl)Cl>[CH3:1][O:2][C:3](=[O:28])/[C:4](/[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[CH2:14][O:15][C:16]1[CH:21]=[CH:20][C:19]([N:22]([CH2:23][CH:24]([CH3:26])[CH3:25])[CH3:31])=[CH:18][C:17]=1[F:27])=[CH:5]/[O:6][CH3:7]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 712FormaldehydeHCID 516892Sodium BicarbonateHCID 5049666Sodium triacetoxyborohydrideHCID 11617976HCID 11617976、化合物

生成物 1

HCID 11596500HCID 11596500、化合物収率 73%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

70 mg (0.18 mmol) of the compound obtained in Step 3 was dissolved in 1.5 ml of methylene chloride, and 57 mg (0.27 mmol) of NaBH(OAc)3 and 30 μl (0.40 mmol) of formaldehyde were added thereto. After stirring at room temperature for 22 hours, the reaction mixture was treated with a saturated sodium bicarbonate aqueous solution, and the water layer was separated and extracted twice with 10 ml of methylene chloride. The organic layers were combined, dried over anhydrous MgSO4, and concentrated under a reduced pressure. The residue was subjected to column chromatography using 20% ethyl acetate/hexane as an eluent to obtain 50 mg (yield 73%) of (E)-methyl-2-[2-((4-(N-isobutyl-N-methylamino)-2-fluorophenoxy)methyl)phenyl]-3-methoxyacrylate as an oil.

後処理

  1. customthe water layer was separated
  2. extractionextracted twice with 10 ml of methylene chloride
  3. dry with materialdried over anhydrous MgSO4
  4. concentrationconcentrated under a reduced pressure

出典と根拠

ORDレコード
ord-0711d64f289d4ba0ab28296c1bb3f391
出典データセット
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08227456B2

反応ノート

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