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Hydrochloric Acid → N-((S)-1-(3,4-dichlorophenyl)-2-hydroxyethyl)-2-(1,1,1-trifluoropropan-2-ylamino)-5,6-dihydropyrido[3,4-d]pyrimidine-7(8H)-carboxamide

HRID 2279540
ノート
印刷プレビュー

反応式

HRID 2279540 の反応式
[Si]([O:8][CH2:9][C@@H:10]([NH:19][C:20]([N:22]1[CH2:31][CH2:30][C:29]2[CH:28]=[N:27][C:26]([NH:32][CH:33]([CH3:38])[C:34]([F:37])([F:36])[F:35])=[N:25][C:24]=2[CH2:23]1)=[O:21])[C:11]1[CH:16]=[CH:15][C:14]([Cl:17])=[C:13]([Cl:18])[CH:12]=1)(C(C)(C)C)(C)C.Cl.CC(O)C>C(Cl)Cl>[Cl:18][C:13]1[CH:12]=[C:11]([C@H:10]([NH:19][C:20]([N:22]2[CH2:31][CH2:30][C:29]3[CH:28]=[N:27][C:26]([NH:32][CH:33]([CH3:38])[C:34]([F:36])([F:37])[F:35])=[N:25][C:24]=3[CH2:23]2)=[O:21])[CH2:9][OH:8])[CH:16]=[CH:15][C:14]=1[Cl:17]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 3776IsopropanolHCID 68294705N-((S)-2-(tert-butyldimethylsilyloxy)-1-(3,4-dichlorophenyl)ethyl)-2-(1,1,1-trifluoropropan-2-ylamino)-5,6-dihydropyrido[3,4-d]pyrimidine-7(8H)-carboxamide

生成物 1

HCID 86705530N-((S)-1-(3,4-dichlorophenyl)-2-hydroxyethyl)-2-(1,1,1-trifluoropropan-2-ylamino)-5,6-dihydropyrido[3,4-d]pyrimidine-7(8H)-carboxamide

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒

実験手順

To a solution of 302 (0.160 g, 0.270 mmol) and DCM (5 mL) at RT was added 6M HCl in IPA (0.450 mL, 2.70 mmol) and the reaction was stirred for 1 h. The reaction was poured into satd. aq. Na2CO3, 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 a DCM/MeOH gradient (500:20 to 500:30) to afford 0.010 g (7.74%) of I-76: MS m/z (APCI-pos) M+1=478.

後処理

  1. additionThe reaction was poured into satd
  2. extractionaq. Na2CO3, and extracted 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 a DCM/MeOH gradient (500:20 to 500:30)
  8. customto afford 0.010 g (7.74%) of I-76

出典と根拠

ORDレコード
ord-b5fd21ac9eab4f3e9e46a1113b9da615
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…

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