Tetrahydrofuran → HCID 178482395、化合物

HRID 450334ノート

反応式

HRID 450334 の反応式
[CH3:1][NH:2][C:3]1[C:11]([N+:12]([O-:14])=[O:13])=[CH:10][C:6]([C:7]([OH:9])=O)=[C:5]([N:15]2[CH2:20][CH2:19][CH:18]([C:21]([F:24])([F:23])[F:22])[CH2:17][CH2:16]2)[N:4]=1.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.[B-](F)(F)(F)F.C1COCC1.[F:52][C:53]([F:62])([F:61])[C@H:54]1[CH2:59][CH2:58][C@H:57]([NH2:60])[CH2:56][CH2:55]1>O.CN(C=O)C>[F:52][C:53]([F:61])([F:62])[C@H:54]1[CH2:55][CH2:56][C@H:57]([NH:60][C:7](=[O:9])[C:6]2[CH:10]=[C:11]([N+:12]([O-:14])=[O:13])[C:3]([NH:2][CH3:1])=[N:4][C:5]=2[N:15]2[CH2:20][CH2:19][CH:18]([C:21]([F:23])([F:24])[F:22])[CH2:17][CH2:16]2)[CH2:58][CH2:59]1

参加物

7

反応物 4

HCID 8028TetrahydrofuranHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 679584096-Methylamino-5-nitro-2-(4-trifluoromethyl-piperidinyl)-nicotinic acidHCID 178511531HCID 178511531、化合物

生成物 1

HCID 178482395HCID 178482395、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 6-methylamino-5-nitro-2-(4-trifluoromethyl-piperidinyl)-nicotinic acid (570 mg, 1.64 mmol), TBTU (540 mg, 1.68 mmol), TEA (1.00 mL, 7.2 mmol), THF (10 mL) and DMF (5 mL) are stirred for 5 min. Then trans-4-trifluoromethyl-cyclohexylamine (335 mg, 1.65 mmol) is added and it is stirred for 30 min. Water is added, the mixture is concentrated and the precipitate is filtered, washed with water and dried at 55° C.

後処理

  1. stirringit is stirred for 30 min
  2. concentrationthe mixture is concentrated
  3. filtrationthe precipitate is filtered
  4. washwashed with water
  5. customdried at 55° C.

出典と根拠

ORDレコード
ord-ef2e87da43b24340965ab2eb288af87d
出典データセット
uspto-grants-2013_07
特許番号
US08486968B2

反応ノート

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