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

1,2-Dichloroethane → HCID 71470591、化合物

HRID 900166
ノート
印刷プレビュー

反応式

HRID 900166 の反応式
[C:1]1([C:7]2[C:15]3[C:14]([NH2:16])=[N:13][CH:12]=[N:11][C:10]=3[NH:9][C:8]=2[Si:17]([CH2:22][CH3:23])([CH2:20][CH3:21])[CH2:18][CH3:19])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(Cl)CCl.C1C=CC2N(O)N=NC=2C=1.[O:38]1[CH2:42][CH2:41][CH2:40][C@H:39]1[C:43](O)=O.[H-].[Al+3].[Li+].[H-].[H-].[H-]>CN(C1C=CN=CC=1)C.CN(C=O)C.C1COCC1.ClCCl>[C:1]1([C:7]2[C:15]3[C:14]([NH:16][CH2:43][C@@H:39]4[CH2:40][CH2:41][CH2:42][O:38]4)=[N:13][CH:12]=[N:11][C:10]=3[NH:9][C:8]=2[Si:17]([CH2:20][CH3:21])([CH2:22][CH3:23])[CH2:18][CH3:19])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=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

10

反応物 5

HCID 111,2-DichloroethaneHCID 757711-HydroxybenzotriazoleHCID 446666Tetrahydro-2-furoic acid, (-)-HCID 21226445Aluminium lithium hydrideHCID 58603334HCID 58603334、化合物

生成物 1

HCID 71470591HCID 71470591、化合物

試薬・触媒・溶媒 4

HCID 14284
4-(Dimethylamino)pyridine
触媒
HCID 6228Dimethylformamide溶媒
HCID 6344Dichloromethane溶媒
HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

To a slurry of 4.00 g (12.3 mmol) of 5-phenyl-6-(triethylsilyl)-7-H-pyrrolo[2,3-d]pyrimidin-4-amine, 3.10 g (16.0 mmol) of EDC and 2.50 g (18.5 mmol) of HOBt and catalytic DMAP in 20 ml DMF was added dropwise 1.91 g (14.8 mmol) of (S)-tetrahydro-2-furoic acid at 0° C. The reaction mixture was stirred at 0° C. for 1 h, then was warmed to room temperature and stirred for 30 h. Dichloromethane (500 ml) was added and the mixture was washed with brine (1×), saturated aqueous sodium bicarbonate (1×), and brine (1×). The organic layer was dried over Na2SO4 and filtered. The crude amide was dissolved in 20 ml THF and added to a solution of 700 mg (27.1 mmol) of lithium aluminum hydride in 40 ml THF at 0° C. The slurry was warmed to room temperature and stirred for 1 h, and then to 50° C. and stirred for an additional 2 h. The reaction mixture was cooled to room temperature and poured into ice water. The aqueous material was extracted with ethyl acetate (4×). The combined organic layers were washed with brine (1×), dried over Na2SO4, filtered and purified by chromatography on silica gel (EtOAc:MeOH:Et3N, 9:1:0.1) to give the title compound. 1H-NMR (400 MHz, CDCl3)δ, 0.61 (q, J=7.6 Hz, 6 H), 0.89 (t, J=7.6 Hz, 9 H), 1.48 (m, 1 H), 1.69-1.85 (m, 3 H), 3.59-3.62 (m, 4 H), 3.94 (m, 1 H), 5.03 (s, 1 H), 7.28 (m, 3 H), 7.45 (m, 2 H), 8.33 (s, 1 H), 8.68 (s, 1 H). Mass Spectrum (ESI) m/e=409.1 (M+1).

後処理

  1. temperaturewas warmed to room temperature
  2. stirringstirred for 30 h
  3. washthe mixture was washed with brine (1×), saturated aqueous sodium bicarbonate (1×), and brine (1×)
  4. dry with materialThe organic layer was dried over Na2SO4
  5. filtrationfiltered
  6. dissolutionThe crude amide was dissolved in 20 ml THF
  7. temperatureThe slurry was warmed to room temperature
  8. stirringstirred for 1 h
  9. stirringto 50° C. and stirred for an additional 2 h
  10. temperatureThe reaction mixture was cooled to room temperature
  11. extractionThe aqueous material was extracted with ethyl acetate (4×)
  12. washThe combined organic layers were washed with brine (1×)
  13. dry with materialdried over Na2SO4
  14. filtrationfiltered
  15. custompurified by chromatography on silica gel (EtOAc:MeOH:Et3N, 9:1:0.1)

出典と根拠

ORDレコード
ord-d8bd987ad3aa46b8a40b3aba8d141d9e
出典データセット
uspto-grants-2008_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07358250B2

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