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Triethylamine → HCID 86612479、化合物

HRID 2080249
ノート
印刷プレビュー

反応式

HRID 2080249 の反応式
[N:1]1[C:10]2[C:5](=[CH:6][C:7](C(O)=O)=[CH:8][CH:9]=2)[CH:4]=[N:3][CH:2]=1.[O:14]([C:21]1[CH:22]=C([CH:26]=[CH:27][CH:28]=1)CN)[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.F[P-](F)(F)(F)(F)F.N1([O:45][P+](N(C)C)(N(C)C)N(C)C)C2C=CC=CC=2N=N1.C([N:58]([CH2:61][CH3:62])[CH2:59]C)C>CN(C)C=O.O>[O:14]([C:21]1[CH:22]=[C:62]([CH:26]=[CH:27][CH:28]=1)[CH2:61][NH:58][C:59]([C:2]1[N:3]=[CH:4][C:5]2[C:10](=[CH:9][CH:8]=[CH:7][CH:6]=2)[N:1]=1)=[O:45])[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=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 8471TriethylamineHCID 151348Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphateHCID 10948363-Phenoxy-benzylamineHCID 23130441Quinazoline-6-carboxylic acid

生成物 1

HCID 86612479HCID 86612479、化合物収率 50%

試薬・触媒・溶媒 2

HCID 962
Water
溶媒
HCID 6228Dimethylformamide溶媒

実験手順

To a solution of quinazoline-6-carboxylic acid obtained in Preparation Example H-3 (9 mg, 0.052 mmol) in N,N-dimethylformamide (3 mL) were added 3-phenoxybenzylamine described in Preparation Example 4 (11 mg, 0.052 mmol), benzotriazol-1-yloxytris(dimethylamino)phosphonium hexafluorophosphate (28 mg, 0.062 mmol) and triethylamine (17 μl, 0.125 mmol), and the solution was stirred for 2 days at room temperature. Water was added to the reaction mixture, which was extracted with ethyl acetate, and concentrated. The residue was purified by NH silica gel column chromatography (hexane-ethyl acetate), and the title compound (11 mg, 0.031 mmol, 50%) was obtained.

後処理

  1. extractionwas extracted with ethyl acetate
  2. concentrationconcentrated
  3. customThe residue was purified by NH silica gel column chromatography (hexane-ethyl acetate)

出典と根拠

ORDレコード
ord-6f0238b59ea74329bbdb42625ef70b5a
出典データセット
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07932272B2

反応ノート

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