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1,2-Dichloroethane → HCID 57888656、化合物

HRID 1820283
ノート
印刷プレビュー

反応式

HRID 1820283 の反応式
[NH2:1][C:2]1[N:7]=[C:6]([C:8]([OH:10])=O)[CH:5]=[CH:4][CH:3]=1.C(Cl)CCl.C1C=CC2N(O)N=NC=2C=1.CCN(C(C)C)C(C)C.Cl.[NH2:35][C@H:36]([CH:55]([CH3:57])[CH3:56])[C:37]([N:39]1[CH2:44][CH2:43][C@@:42]([C:46]2[CH:51]=[CH:50][C:49]([Cl:52])=[CH:48][CH:47]=2)([OH:45])[C:41]([CH3:54])([CH3:53])[CH2:40]1)=[O:38]>CN(C=O)C>[NH2:1][C:2]1[N:7]=[C:6]([C:8]([NH:35][C@H:36]([CH:55]([CH3:57])[CH3:56])[C:37]([N:39]2[CH2:44][CH2:43][C@@:42]([C:46]3[CH:47]=[CH:48][C:49]([Cl:52])=[CH:50][CH:51]=3)([OH:45])[C:41]([CH3:53])([CH3:54])[CH2:40]2)=[O:38])=[O:10])[CH:5]=[CH:4][CH:3]=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 5

HCID 111,2-DichloroethaneHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 3516526-Aminopyridine-2-carboxylic acidHCID 67299922HCID 67299922、化合物

生成物 1

HCID 57888656HCID 57888656、化合物収率 78.2%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a suspension of 6-aminopicolinic acid (33 mg, 0.24 mmol) in DMF (2 mL) was added EDC (45.9 mg, 0.24 mmol), HOBt (32.3 mg, 0.24 mmol). The mixture was stirred at rt for 0.5 h, then was added DIPEA (0.083 mL, 0.48 mmol) and (R)-2-amino-1-((S)-4-(4-chlorophenyl)-4-hydroxy-3,3-dimethylpiperidin-1-yl)-3-methylbutan-1-one hydrochloride (90 mg, 0.239 mmol). The mixture was stirred at rt overnight. The reaction was quenched with NaHCO3 (aq) and stirred at rt for 1 h, extracted by EtOAc, washed with brine and dried over Na2SO4. After concentrating in vacuo, the residue was triturated with CH2Cl2 and filtered to give a yellow solid as 6-amino-N—((R)-1-((S)-4-(4-chlorophenyl)-4-hydroxy-3,3-dimethylpiperidin-1-yl)-3-methyl-1-oxobutan-2-yl)picolinamide (86 mg, 0.187 mmol, 78% yield).

後処理

  1. stirringThe mixture was stirred at rt overnight
  2. customThe reaction was quenched with NaHCO3 (aq)
  3. stirringstirred at rt for 1 h
  4. extractionextracted by EtOAc
  5. washwashed with brine
  6. dry with materialdried over Na2SO4
  7. concentrationAfter concentrating in vacuo
  8. customthe residue was triturated with CH2Cl2
  9. filtrationfiltered

出典と根拠

ORDレコード
ord-266fea61655c4a9c9aa639825f541a88
出典データセット
uspto-grants-2009_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07601844B2

反応ノート

読み込み中…

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