Triphenylphosphine → HCID 117729706、化合物

HRID 60628

反応式

HRID 60628 の反応式
[NH2:1][C:2]1[N:6]([C:7]2[CH:8]=[CH:9][C:10]([Cl:14])=[C:11]([OH:13])[CH:12]=2)[N:5]=[C:4]([C:15]([CH3:18])([CH3:17])[CH3:16])[CH:3]=1.[O:19]1[CH2:24][CH2:23][N:22]([CH:25](O)[CH3:26])[CH2:21][CH2:20]1.C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.CCOC(/N=N/C(OCC)=O)=O>C1COCC1.O>[C:15]([C:4]1[CH:3]=[C:2]([NH2:1])[N:6]([C:7]2[CH:8]=[CH:9][C:10]([Cl:14])=[C:11]([O:13][CH2:26][CH2:25][N:22]3[CH2:23][CH2:24][O:19][CH2:20][CH2:21]3)[CH:12]=2)[N:5]=1)([CH3:18])([CH3:17])[CH3:16]

参加物

7

反応物 4

HCID 11776TriphenylphosphineHCID 30293761-MorpholinoethanolHCID 5462977Diethyl azodicarboxylateHCID 689526455-(5-amino-3-tert-butyl-1H-pyrazol-1-yl)-2-chlorophenol

生成物 1

HCID 117729706HCID 117729706、化合物収率 80%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a stirred solution of 5-(5-amino-3-tert-butyl-pyrazol-1-yl)-2-chloro-phenol (WO2007/091152, which is incorporated herein by reference; 200 mg, 0.75 mmol), 2-N morpholino ethanol (137 μL, 1.13 mmol) and Ph3P (394 mg, 1.50 mmol) in THF (7.5 mL) at 0° C. was added DEAD (236 μL, 1.50 mmol). After 1 h, the reaction mixture was diluted with water and extracted with DCM. The combined organics were dried and concentrated in vacuo. The residue was purified by FCC, using 0-5% [2M NH3 in MeOH] in DCM, to give the title compound (228 mg, 80%). LCMS (Method 3): Rt 2.28 min, m/z 379 [MH+].

後処理

  1. extractionextracted with DCM
  2. customThe combined organics were dried
  3. concentrationconcentrated in vacuo
  4. customThe residue was purified by FCC

出典と根拠

ORDレコード
ord-a8c53b9729bd4bf6ae02d50abae60ae2
出典データセット
uspto-grants-2016_09
特許番号
US09440974B2

関連ノート

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