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Triphenylphosphine → HCID 178454107、化合物

HRID 707291
ノート
印刷プレビュー

反応式

HRID 707291 の反応式
[C:1]([O:5][C:6](=[O:13])[NH:7][C@H:8]1[CH2:11][C@H:10](O)[CH2:9]1)([CH3:4])([CH3:3])[CH3:2].[Br:14][C:15]1[N:20]=[C:19]2[N:21]([CH:25]3[CH2:27][CH2:26]3)[C:22](=[O:24])[NH:23][C:18]2=[N:17][CH:16]=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>C1COCC1>[C:1]([O:5][C:6](=[O:13])[NH:7][C@H:8]1[CH2:11][C@H:10]([N:23]2[C:18]3=[N:17][CH:16]=[C:15]([Br:14])[N:20]=[C:19]3[N:21]([CH:25]3[CH2:26][CH2:27]3)[C:22]2=[O:24])[CH2:9]1)([CH3:4])([CH3:3])[CH3:2]
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 11776TriphenylphosphineHCID 5363146Diisopropyl azodicarboxylateHCID 86694158HCID 86694158、化合物HCID 178454126HCID 178454126、化合物

生成物 1

HCID 178454107HCID 178454107、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a cooled (0° C.) solution of tert-butyl(trans-3-hydroxycyclobutyl)carbamate (0.250 g, 1.335 mmol), 6-bromo-1-cyclopropyl-1H-imidazo[4,5-b]pyrazin-2(3H)-one (0.334 g, 1.309 mmol) and triphenylphosphine (0.520 g, 1.983 mmol) in THF (10 ml) was added DIAD (0.400 ml, 2.032 mmol) dropwise via syringe. After 10 min the reaction was allowed to warm to room temperature and stirred overnight. The reaction mixture was concentrated in vacuo and the residue was dissolved in MeOH/EtOAc, evaporated onto silica gel and purified by flash chromatography (Isco (25 gram)) eluting with EtOAc:hexanes (0:1-1:1) to give a light-yellow solid. ESI MS 445.9, 447.8 [M+Na].

後処理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. dissolutionthe residue was dissolved in MeOH/EtOAc
  3. customevaporated onto silica gel
  4. custompurified by flash chromatography (Isco (25 gram))
  5. washeluting with EtOAc:hexanes (0:1-1:1)
  6. customto give a light-yellow solid

出典と根拠

ORDレコード
ord-49e03840244c436e8fd6f5eedd8fc8bb
出典データセット
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09174992B2

反応ノート

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