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Triphenylphosphine → HCID 68313033、化合物

HRID 1530387
ノート
印刷プレビュー

反応式

HRID 1530387 の反応式
[CH2:1]([O:8][C:9]([N:11]1[CH2:16][CH2:15][CH:14]([CH:17]([O:20][C:21]2[CH:43]=[CH:42][C:24]3[C:25]4[N:29]([CH2:30][CH2:31][O:32][C:23]=3[CH:22]=2)[CH:28]=[C:27]([C:33]2[N:34]([CH:39]([CH3:41])[CH3:40])[N:35]=[C:36]([CH3:38])[N:37]=2)[N:26]=4)[CH2:18]C)[CH2:13][CH2:12]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(OC(N1CCC(C(O)C)CC1)=O)C1C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.CC(OC(/N=N/C(OC(C)C)=O)=O)C>O1CCOCC1.CCOC(C)=O>[CH2:1]([O:8][C:9]([N:11]1[CH2:12][CH2:13][CH:14]([CH:17]([O:20][C:21]2[CH:43]=[CH:42][C:24]3[C:25]4[N:29]([CH2:30][CH2:31][O:32][C:23]=3[CH:22]=2)[CH:28]=[C:27]([C:33]2[N:34]([CH:39]([CH3:40])[CH3:41])[N:35]=[C:36]([CH3:38])[N:37]=2)[N:26]=4)[CH3:18])[CH2:15][CH2:16]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 11776TriphenylphosphineHCID 5363146Diisopropyl azodicarboxylateHCID 18918437Phenylmethyl 4-(1-hydroxyethyl)-1-piperidinecarboxylateHCID 68312705HCID 68312705、化合物

生成物 1

HCID 68313033HCID 68313033、化合物収率 20%

試薬・触媒・溶媒 2

HCID 8857
Ethyl Acetate
溶媒
HCID 312751,4-Dioxane溶媒

実験手順

To a suspension of 2-(2-isopropyl-5-methyl-2H-[1,2,4]triazol-3-yl)-4,5-dihydro-6-oxa-1,3a-diazabenzo[e]azulen-8-ol from Example 4 (400 mg, 1.23 mmol), 4-(1-hydroxyethyl)piperidine-1-carboxylic acid benzyl ester (487 mg, 1.85 mmol) and triphenylphosphine (548 mg, 2.09 mmol) in dioxane (7 mL) was added dropwise DIAD (410 ul, 2.09 mmol) and the reaction mixture was stirred at RT for 18 h. The mixture was then diluted with EtOAc and washed with aq. NaOH (1N). The aqueous phase was extracted with EtOAc (×3) and the combined organic layers were then washed with brine, dried over MgSO4 and concentrated in vacuo. The resulting residue was purified by column chromatography (Si-PCC, gradient 0-10% MeOH in EtOAc), then suspended in DCM and filtered. The filtrate was concentrated in vacuo and purified by column chromatography (Si-PCC, gradient 0-10% MeOH in DCM) affording 4-{1-[2-(2-Isopropyl-5-methyl-2H-[1,2,4]triazol-3-yl)-4,5-dihydro-6-oxa-1,3a-diazabenzo[e]azulen-8-yloxy]ethyl}piperidine-1-carboxylic acid benzyl ester (140 mg, 20%). LCMS: RT 3.90 min [M+H]+ 571.0

後処理

  1. washwashed with aq. NaOH (1N)
  2. extractionThe aqueous phase was extracted with EtOAc (×3)
  3. washthe combined organic layers were then washed with brine
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated in vacuo
  6. customThe resulting residue was purified by column chromatography (Si-PCC, gradient 0-10% MeOH in EtOAc)
  7. filtrationfiltered
  8. concentrationThe filtrate was concentrated in vacuo
  9. custompurified by column chromatography (Si-PCC, gradient 0-10% MeOH in DCM)

出典と根拠

ORDレコード
ord-12956316429545abb718aee1a48d4a17
出典データセット
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09090628B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート