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Water → HCID 57635145、化合物

HRID 2110199
ノート
印刷プレビュー

反応式

HRID 2110199 の反応式
[CH3:1][C:2]([CH3:30])([CH3:29])[C@H:3]([NH:8][C:9]([C:11]1[N:12]=[C:13]([C:21]#[C:22][C:23]2[CH:28]=[CH:27]C=CC=2)[N:14]2[CH2:19][CH2:18][N:17]([CH3:20])[CH2:16][C:15]=12)=[O:10])[C:4]([NH:6][CH3:7])=[O:5].C1(B(O)O)CCCC=1.C(=O)([O-])[O-].[K+].[K+].O>O1CCOCC1.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[C:21]1([C:13]2[N:14]3[CH2:19][CH2:18][N:17]([CH3:20])[CH2:16][C:15]3=[C:11]([C:9]([NH:8][C@@H:3]([C:2]([CH3:1])([CH3:29])[CH3:30])[C:4]([NH:6][CH3:7])=[O:5])=[O:10])[N:12]=2)[CH2:27][CH2:28][CH2:23][CH:22]=1
参加物反応条件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 962WaterHCID 11430Potassium CarbonateHCID 3861343(Cyclopent-1-en-1-yl)boronic acidHCID 57635127HCID 57635127、化合物

生成物 1

HCID 57635145HCID 57635145、化合物

試薬・触媒・溶媒 2

HCID 178418397HCID 178418397、化合物
触媒
HCID 312751,4-Dioxane溶媒

反応条件

温度
100 °C

実験手順

Compound 203 (100 mg, 0.26 mmol) was dissolved in dioxane (2 mL) and cyclopentenylboronic acid (58 mg, 0.52 mmol) was added, followed by potassium carbonate (72 mg, 0.52 mmol) and water (0.40 mL). The resulting solution was degassed with nitrogen gas and Pd(PPh3)4 (18 mg, 0.016 mmol) was added. The mixture was heated at 100° C. for 1 h under nitrogen. The organic layer was separated, solid NaCl was added and the mixture was extracted with ethyl acetate. The combined organic layers were filtered through PL-Thiol MP SPE tube to remove palladium catalyst. The filtrate was concentrated and then purified by prep LC/MS using 5-95% acetonitrile in water with 0.1% formic acid. The formic acid was removed using Strata SCX SPE tube to give a desired product (Compound 238) as a free base (81 mg, 82%). 1H-NMR (400 MHz, CDCl3) δ: 1.09 (s, 9H), 1.90-2.05 (m, 2H), 2.51 (s, 3H), 2.55-2.65 (m, 2H), 2.74-2.95 (m, 7H), 3.88-4.14 (m, 4H), 5.95 (s, 1H), 6.09 (m, 1H), 7.66 (d, 1H). LCMS (+ESI) m/z 374.2 [M+H]+.

後処理

  1. additionwas added
  2. customThe organic layer was separated
  3. additionsolid NaCl was added
  4. extractionthe mixture was extracted with ethyl acetate
  5. filtrationThe combined organic layers were filtered through PL-Thiol MP SPE tube
  6. customto remove palladium catalyst
  7. concentrationThe filtrate was concentrated
  8. custompurified by prep LC/MS
  9. customThe formic acid was removed

出典と根拠

ORDレコード
ord-7a657b99e7294ce0bf0691c51667c8d7
出典データセット
uspto-grants-2009_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07517874B2

反応ノート

読み込み中…

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