Dimethylformamide → HCID 89672302、化合物

HRID 40498

反応式

HRID 40498 の反応式
[NH:1]1[CH:5]=[C:4]([C:6]([OH:8])=O)[CH:3]=[N:2]1.CN(C=O)C.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.[B-](F)(F)(F)F.[Br:36][C:37]1[CH:42]=[CH:41][C:40]([C@@H:43]([NH2:45])[CH3:44])=[CH:39][CH:38]=1>>[Br:36][C:37]1[CH:42]=[CH:41][C:40]([C@@H:43]([NH:45][C:6]([C:4]2[CH:3]=[N:2][NH:1][CH:5]=2)=[O:8])[CH3:44])=[CH:39][CH:38]=1

参加物

5

反応物 4

HCID 6228DimethylformamideHCID 852999(alphaS)-4-Bromo-alpha-methylbenzenemethanamineHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 3015937Pyrazole-4-carboxylic acid

生成物 1

HCID 89672302HCID 89672302、化合物

実験手順

To 5.0 g (44.6 mmol) 4-pyrazolecarboxylic acid in 100 mL DMF 15.2 mL (89.2 mmol) DIPEA and 15.7 g (49.1 mmol) TBTU are added and the mixture is stirred for 10 min at rt. Subsequently 8.9 g (44.6 mmol) (S)-1-(4-bromophenyl)ethylamine are added and stirring is continued over night. The mixture is poured on water and is extracted with ethyl acetate. The combined organic layers are dried over sodium sulphate and the solvent is removed in vacuo. The residue is triturated with DCM to yield the desired product.

後処理

  1. stirringstirring
  2. waitis continued over night
  3. additionThe mixture is poured on water
  4. extractionis extracted with ethyl acetate
  5. dry with materialThe combined organic layers are dried over sodium sulphate
  6. customthe solvent is removed in vacuo
  7. customThe residue is triturated with DCM

出典と根拠

ORDレコード
ord-35c558e166d3439c925f4ad65b21b742
出典データセット
uspto-grants-2013_09
特許番号
US08530461B2

関連ノート

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