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Triethylamine → HCID 58550869、化合物

HRID 2204253
ノート
印刷プレビュー

反応式

HRID 2204253 の反応式
[CH2:1]([C:3]1[CH:11]=[CH:10][C:6]([C:7]([OH:9])=O)=[CH:5][C:4]=1[O:12][CH3:13])[CH3:2].CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[CH:38]1[N:46]2[C:41]([C:42]3([CH2:59][CH2:58][NH:57][CH2:56][CH2:55]3)[O:43][C:44]3[CH:50]=[C:49]([C:51]([O:53][CH3:54])=[O:52])[CH:48]=[CH:47][C:45]=32)=[CH:40][CH:39]=1.CCN(CC)CC>CN(C=O)C.C(OCC)(=O)C>[CH2:1]([C:3]1[CH:11]=[CH:10][C:6]([C:7]([N:57]2[CH2:58][CH2:59][C:42]3([O:43][C:44]4[CH:50]=[C:49]([C:51]([O:53][CH3:54])=[O:52])[CH:48]=[CH:47][C:45]=4[N:46]4[CH:38]=[CH:39][CH:40]=[C:41]34)[CH2:55][CH2:56]2)=[O:9])=[CH:5][C:4]=1[O:12][CH3:13])[CH3:2]
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 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 299406594-Ethyl-3-methoxybenzoic acidHCID 58551707HCID 58551707、化合物

生成物 1

HCID 58550869HCID 58550869、化合物収率 95.5%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

A solution of 4-ethyl-3-methoxy-benzoic acid (450 mg, 2.5 mmol), HATU (940 mg, 2.5 mmol), methyl spiro[piperidine-4,4′-pyrrolo[2,1-c][1,4]benzoxazine]-7′-carboxylate (830 mg, 2.5 mmol), and Et3N (1.7 mL, 9.9 mmol) in DMF (8 mL) was stirred at room temperature overnight. The reaction was diluted with ethyl acetate and washed with saturated sodium bicarbonate solution. The organics were dried over sodium sulfate, filtered and evaporated to yield a crude mixture that was purified by silica gel chromatography eluting with 0-30% EtOAc in hexanes to yield methyl 1′-(4-ethyl-3-methoxybenzoyl)spiro[benzo[b]pyrrolo[1,2-d][1,4]oxazine-4,4′-piperidine]-7-carboxylate (1.1 g, quant). ESI-MS m/z calc. 460.5, found 461.5 (M+1)+; Retention time: 2.08 minutes (3 min run).

後処理

  1. washwashed with saturated sodium bicarbonate solution
  2. dry with materialThe organics were dried over sodium sulfate
  3. filtrationfiltered
  4. customevaporated
  5. customto yield a crude mixture that
  6. customwas purified by silica gel chromatography
  7. washeluting with 0-30% EtOAc in hexanes

出典と根拠

ORDレコード
ord-9066f6b054a845f09297492fbe63fc94
出典データセット
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09365588B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート