ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Hydrochloric Acid → HCID 178422168、化合物

HRID 2095736
ノート
印刷プレビュー

反応式

HRID 2095736 の反応式
Br[C:2]1[CH:3]=[C:4]2[C:10]([C@@H:11]([C:13]3[C:18]([OH:19])=[CH:17][CH:16]=[C:15]([F:20])[C:14]=3[Cl:21])[CH3:12])=[CH:9][N:8](C(OC(C)(C)C)=O)[C:5]2=[N:6][CH:7]=1.C([O-])([O-])=O.[K+].[K+].CN(C=O)C.[CH:40](I)([CH3:42])[CH3:41].[CH3:44][C:45]1[N:49]([C@H:50]2[CH2:55][CH2:54][C@H:53]([OH:56])[CH2:52][CH2:51]2)[N:48]=[CH:47][C:46]=1B1OC(C)(C)C(C)(C)O1.O.Cl>CCOC(C)=O.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.O1CCOCC1>[Cl:21][C:14]1[C:15]([F:20])=[CH:16][CH:17]=[C:18]([O:19][CH:40]([CH3:42])[CH3:41])[C:13]=1[C@H:11]([C:10]1[C:4]2[C:5](=[N:6][CH:7]=[C:2]([C:46]3[CH:47]=[N:48][N:49]([C@H:50]4[CH2:55][CH2:54][C@H:53]([OH:56])[CH2:52][CH2:51]4)[C:45]=3[CH3:44])[CH:3]=2)[NH:8][CH:9]=1)[CH3:12]
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

11

反応物 7

HCID 313Hydrochloric AcidHCID 962Water2 回HCID 6228DimethylformamideHCID 6362Isopropyl iodideHCID 11430Potassium Carbonate2 回HCID 67003938tert-butyl 5-bromo-3-[(1S)-1-(2-chloro-3-fluoro-6-hydroxyphenyl)ethyl]-1H-pyrrolo[2,3-b]pyridine-1-carboxylate
HCID 178421686
HCID 178421686、化合物

生成物 1

HCID 178422168HCID 178422168、化合物

試薬・触媒・溶媒 3

HCID 178418397HCID 178418397、化合物触媒HCID 8857Ethyl Acetate溶媒HCID 312751,4-Dioxane溶媒

反応条件

温度
40 °C

実験手順

To a solution of tert-butyl 5-bromo-3-[(1S)-1-(2-chloro-3-fluoro-6-hydroxyphenyl)ethyl]-1H-pyrrolo[2,3-b]pyridine-1-carboxylate (13.0 mg, 0.0277 mmol) and K2CO3 (12.7 mg, 0.0919 mmol) in DMF (0.8 mL, 10 mmol) was added isopropyl iodide (16.06 mg, 0.09451 mmol), and the mixture was heated to 40° C. for 2 h. The reaction mixture was diluted with EtOAc and washed with water (3×). The organic layer was concentrated in vacuo, and trans-4-[5-methyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazol-1-yl]cyclohexanol (12.71 mg, 0.04151 mmol), Pd(PPh3)4 (1.599 mg, 0.001384 mmol), K2CO3 (3 eq) and 4:1 dioxane:H2O (1 mL, 10 mmol) were added. The mixture was heated in a microwave reactor at 95° C. for 20 min. 12 M of HCl in H2O (0.069 mL, 0.83 mmol) was added, and the solution was heated to 45° C. for 1 h. The solution was used directly for HPLC purification, and the fractions containing the pure product were concentrated in vacuo to afford the title compound as a white solid. 1H NMR (400 MHz, CD3OD): δ=0.68 (br. s., 3H), 1.24 (d, J=5.8 Hz, 3H), 1.45-1.57 (m, 2H), 1.80 (d, J=7.1 Hz, 3H), 1.94-2.11 (m, 6H), 2.19 (s, 3H), 3.68 (tt, J=11.0, 4.2 Hz, 1H), 4.12-4.24 (m, 1H), 4.35-4.51 (m, 1H), 5.01-5.12 (m, 1H), 6.83 (dd, J=8.3, 3.8 Hz, 1H), 7.05 (t, J=8.8 Hz, 1H), 7.33 (dd, J=2.9, 1.6 Hz, 2H), 7.45 (s, 1H), 8.09 (d, J=2.0 Hz, 1H). MS (ES+): m/z=511.34/513.33 (100/50) [MH+]. HPLC: tR=1.33 min (polar—2 min, UPLC-ACQUITY).

後処理

  1. washwashed with water (3×)
  2. temperatureThe mixture was heated in a microwave reactor at 95° C. for 20 min
  3. temperaturethe solution was heated to 45° C. for 1 h
  4. customThe solution was used directly for HPLC purification
  5. additionthe fractions containing the pure product
  6. concentrationwere concentrated in vacuo

出典と根拠

ORDレコード
ord-a4859c677cf0435aa46aa14d8d34a8da
出典データセット
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08445510B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート