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tert-Butanol → (4-Benzyloxy-6-methoxy-[1,5]naphthyridin-3-yl)-carbamic acid tert-butyl ester

HRID 2273235
ノート
印刷プレビュー

反応式

HRID 2273235 の反応式
C1(P(N=[N+]=[N-])(C2C=CC=CC=2)=[O:8])C=CC=CC=1.[CH2:18]([O:25][C:26]1[C:35]2[C:30](=[CH:31][CH:32]=[C:33]([O:36][CH3:37])[N:34]=2)[N:29]=[CH:28][C:27]=1C(O)=O)[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.[C:41]([OH:45])([CH3:44])([CH3:43])[CH3:42].C([N:48]([CH2:51]C)CC)C>CN(C)C=O>[C:41]([O:45][C:51](=[O:8])[NH:48][C:27]1[CH:28]=[N:29][C:30]2[C:35]([C:26]=1[O:25][CH2:18][C:19]1[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1)=[N:34][C:33]([O:36][CH3:37])=[CH:32][CH:31]=2)([CH3:44])([CH3:43])[CH3:42]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6386tert-ButanolHCID 8471TriethylamineHCID 199401P,P-Diphenylphosphinic azideHCID 672550274-Benzyloxy-6-methoxy-[1,5]naphthyridine-3-carboxylic acid

生成物 1

HCID 67255694(4-Benzyloxy-6-methoxy-[1,5]naphthyridin-3-yl)-carbamic acid tert-butyl ester

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

反応条件

温度
100 °C

実験手順

Diphenylphosphoryl azide (25.0 mL, 116.0 mmol, 1.5 eq) is added at room temperature to a stirred solution of 4-benzyloxy-6-methoxy-[1,5]naphthyridine-3-carboxylic acid (24.0 g, 77.34 mmol, 1.0 eq) in N,N-dimethylformamide (300 mL), followed by tert-butanol (8.5 mL, 89.71 mmol, 1.16 eq) and triethylamine (104.5 mL, 773.4 mmol, 10.0 eq). After 30 minutes stirring at 70° C. and 2 hours at 100° C., the reaction mixture is cooled down to room temperature, solvent is removed and the residue is extracted with ethyl acetate (3×200 mL) and a saturated sodium hydrogen carbonate aqueous solution (200 mL). The combined organic layers are dried over sodium sulfate, filtered and concentrated to afford crude (4-benzyloxy-6-methoxy-[1,5]naphthyridin-3-yl)-carbamic acid tert-butyl ester that is directly engaged in the next step.

後処理

  1. temperaturethe reaction mixture is cooled down to room temperature
  2. customsolvent is removed
  3. extractionthe residue is extracted with ethyl acetate (3×200 mL)
  4. dry with materialThe combined organic layers are dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-3bcfd68865c24fb8b2146bd07110ea01
出典データセット
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09120822B2

反応ノート

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