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Sodium Carbonate → HCID 59738189、化合物

HRID 561238
ノート
印刷プレビュー

反応式

HRID 561238 の反応式
Br[C:2]1[CH:3]=[CH:4][C:5]([Cl:29])=[C:6]([CH:28]=1)[O:7][CH:8]1[CH2:13][CH2:12][N:11]([C:14]2[CH:18]=[C:17]([C:19]3[N:20]=[N:21][N:22]([CH2:24][C:25]([OH:27])=[O:26])[N:23]=3)[O:16][N:15]=2)[CH2:10][CH2:9]1.[F:30][C:31]([F:43])([F:42])[O:32][C:33]1[CH:38]=[CH:37][C:36](B(O)O)=[CH:35][CH:34]=1.C([O-])([O-])=O.[Na+].[Na+]>C1(C)C=CC=CC=1.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>[Cl:29][C:5]1[CH:4]=[CH:3][C:2]([C:36]2[CH:35]=[CH:34][C:33]([O:32][C:31]([F:30])([F:42])[F:43])=[CH:38][CH:37]=2)=[CH:28][C:6]=1[O:7][CH:8]1[CH2:13][CH2:12][N:11]([C:14]2[CH:18]=[C:17]([C:19]3[N:20]=[N:21][N:22]([CH2:24][C:25]([OH:27])=[O:26])[N:23]=3)[O:16][N:15]=2)[CH2:10][CH2:9]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

6

反応物 3

HCID 10340Sodium CarbonateHCID 27343864-(Trifluoromethoxy)phenylboronic acidHCID 24988884HCID 24988884、化合物

生成物 1

HCID 59738189HCID 59738189、化合物

試薬・触媒・溶媒 2

HCID 178418397HCID 178418397、化合物触媒HCID 1140
Toluene
溶媒

反応条件

温度
80 °C

実験手順

To a suspension of (5-{3-[4-(5-bromo-2-chlorophenoxy)piperidin-1-yl]isoxazol-5-yl}-2H-tetrazol-2-yl)acetic acid (130 mg, 0.269 mmol), [4-(trifluoromethoxy)phenyl]boronic acid (98 mg, 0.476 mmol) and Pd(Ph3P)4 (25 mg, 0.022 mmol) in toluene (4 mL) was added aqueous 2 M Na2CO3 (1.5 mL, 3.00 mmol). After the resulting heterogeneous mixture was purged with nitrogen, it was gently heated to 80° C. for 6 h with stirring under a nitrogen atmosphere. After cooling to room temperature, the reaction was poured into aqueous 1 N HCl and extracted with EtOAc. The organic layer was washed with brine and dried (Na2SO4). Solvents were removed under reduced pressure and the crude material was purified by column chromatography on silica gel (gradient from 0% to 3% HOAc/EtOAc). After concentration, the white solid was co-evaporated twice and triturated with Et2O/heptane to give the title compound as a white solid. 1H NMR (400 MHz, DMSO-d6): δ13.92 (br s, 1H), 7.88-7.83 (m, 2H), 7.57-7.54 (m, 2H), 7.49 (d, 2H), 7.30 (dd, 1H), 7.27 (s, 1H), 5.83 (s, 2H), 5.00-4.93 (m, 1H), 3.68-3.60 (m, 2H), 3.41-3.35 (m, 2H), 2.12-2.02 (s, 2H), 1.87-1.78 (m, 2H). MS: m/z 565 (MH+).

後処理

  1. customAfter the resulting heterogeneous mixture was purged with nitrogen, it
  2. temperatureAfter cooling to room temperature
  3. additionthe reaction was poured into aqueous 1 N HCl
  4. extractionextracted with EtOAc
  5. washThe organic layer was washed with brine
  6. dry with materialdried (Na2SO4)
  7. customSolvents were removed under reduced pressure
  8. customthe crude material was purified by column chromatography on silica gel (gradient from 0% to 3% HOAc/EtOAc)
  9. concentrationAfter concentration
  10. customtriturated with Et2O/heptane

出典と根拠

ORDレコード
ord-2f22af56542a47fe9855fa79c585b553
出典データセット
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08063224B2

反応ノート

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