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Dimethylformamide → (R)-(4-(4-chlorophthalazin-1-yl)-3-methylpiperazin-1-yl)(4,4-difluorocyclohexyl)methanone

HRID 1689976
ノート
印刷プレビュー

反応式

HRID 1689976 の反応式
[F:1][C:2]1([F:11])[CH2:7][CH2:6][CH:5]([C:8]([OH:10])=O)[CH2:4][CH2:3]1.O=C1N(P(Cl)(N2CCOC2=O)=O)CCO1.CN(C=O)C.[Cl:32][C:33]1[C:42]2[C:37](=[CH:38][CH:39]=[CH:40][CH:41]=2)[C:36]([N:43]2[CH2:48][CH2:47][NH:46][CH2:45][C@H:44]2[CH3:49])=[N:35][N:34]=1>C(OCC)(=O)C.C(N(CC)CC)C>[Cl:32][C:33]1[C:42]2[C:37](=[CH:38][CH:39]=[CH:40][CH:41]=2)[C:36]([N:43]2[CH2:48][CH2:47][N:46]([C:8]([CH:5]3[CH2:4][CH2:3][C:2]([F:1])([F:11])[CH2:7][CH2:6]3)=[O:10])[CH2:45][C@H:44]2[CH3:49])=[N:35][N:34]=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 6228DimethylformamideHCID 152842Bis(2-oxo-3-oxazolidinyl)phosphinic chlorideHCID 27791364,4-Difluorocyclohexanecarboxylic acidHCID 57581473(R)-1-chloro-4-(2-methylpiperazin-1-yl)phthalazine

生成物 1

HCID 57581526(R)-(4-(4-chlorophthalazin-1-yl)-3-methylpiperazin-1-yl)(4,4-difluorocyclohexyl)methanone

試薬・触媒・溶媒 2

HCID 8471
Triethylamine
溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

4,4-difluorocyclohexanecarboxylic acid (386 mg, 2.35 mmol) and bis(2-oxo-3-oxazolidinyl)phosphinic chloride (624 mg, 2.45 mmol), DMF (4 mL), and triethylamine (0.57 mL) were stirred at RT for 2 minutes. (R)-1-chloro-4-(2-methylpiperazin-1-yl)phthalazine (JK-2) (537 mg, 2.04 mmol) was added and the reaction stirred at rt for 24 hours. The reaction was then taken up in ethyl acetate (80 mL), washed with aqueous K2CO3 (10%), water, and then saturated sodium chloride. The organics were dried (MgSO4) and evaporated to give a brown oil. Chromatography over silica gel with a gradient of hexanes/0-70% ethyl acetate gave an off-white solid, JK-27. MS (M+H)+=409.1

後処理

  1. washwashed with aqueous K2CO3 (10%), water
  2. dry with materialThe organics were dried (MgSO4)
  3. customevaporated
  4. customto give a brown oil

出典と根拠

ORDレコード
ord-1245ce1632f943169786b7a0077996c3
出典データセット
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08153633B2

反応ノート

読み込み中…

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