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1,1'-Carbonyldiimidazole → HCID 60198533、化合物

HRID 2279507
ノート
印刷プレビュー

反応式

HRID 2279507 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C@H:8]([NH:12][C:13]([N:15]2[CH2:24][C:23]([F:26])([F:25])[C:22]3[CH:21]=[N:20][C:19]([NH:27][CH:28]4[CH2:33][CH2:32][O:31][CH2:30][CH2:29]4)=[N:18][C:17]=3[CH2:16]2)=[O:14])[CH2:9]OC)=[CH:4][C:3]=1F.[Cl:35]C1C=CC([C@H](N)COC)=CC=1F.C1N=CN(C(N2C=NC=C2)=O)C=1.Cl.FC1(F)C2C=NC(NC3CCOCC3)=NC=2CNC1>O.C(Cl)Cl>[Cl:35][C:3]1[CH:4]=[C:5]([C@H:8]([NH:12][C:13]([N:15]2[CH2:24][C:23]([F:25])([F:26])[C:22]3[CH:21]=[N:20][C:19]([NH:27][CH:28]4[CH2:29][CH2:30][O:31][CH2:32][CH2:33]4)=[N:18][C:17]=3[CH2:16]2)=[O:14])[CH3:9])[CH:6]=[CH:7][C:2]=1[Cl:1]
参加物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 682631,1'-CarbonyldiimidazoleHCID 86705500HCID 86705500、化合物HCID 86705502HCID 86705502、化合物HCID 86705503HCID 86705503、化合物

生成物 1

HCID 60198533HCID 60198533、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 6344
Dichloromethane
溶媒
2 回

実験手順

(S)—N-(1-(4-chloro-3-fluorophenyl)-2-methoxyethyl)-5,5-difluoro-2-(tetrahydro-2H-pyran-4-ylamino)-5,6-dihydropyrido[3,4-d]pyrimidine-7(8H)-carboxamide (I-51) To a solution of 197 (0.0854 g, 0.293 mmol) and DCM (5 mL) was added sequentially TEA (0.123 mL, 0.880 mmol) and CDI (0.0476 g, 0.293 mmol) and the solution was stirred at RT for 30 min. To the solution was added dropwise a solution of TEA (0.123 mL, 0.880 mmol), 208 (0.090 g, 0.293 mmol) and DCM (5 mL). The reaction was stirred for 18 h then poured into water and extracted with DCM. The combined organic extracts were dried (MgSO4), filtered, and concentrated in vacuo. The crude product was purified by SiO2 chromatography eluting with 2% MeOH/DCM to afford 0.060 g (40.9%) of I-51: MS m/z (APCI-pos) M+1=499.

後処理

  1. stirringThe reaction was stirred for 18 h
  2. extractionextracted with DCM
  3. dry with materialThe combined organic extracts were dried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe crude product was purified by SiO2 chromatography
  7. washeluting with 2% MeOH/DCM
  8. customto afford 0.060 g (40.9%) of I-51

出典と根拠

ORDレコード
ord-7c1eb5642099408dbe4e86aed027ccf2
出典データセット
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09133187B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート