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4-Tert-Butylaniline → 3-Phenyl-1-oxa-2-azaspiro[4.5]dec-2-ene-8-carboxylic acid-(4-tert-butylphenyl)amide

HRID 1013341
ノート
印刷プレビュー

反応式

HRID 1013341 の反応式
[C:1]1([C:7]2[CH2:11][C:10]3([CH2:16][CH2:15][CH:14]([C:17]([OH:19])=O)[CH2:13][CH2:12]3)[O:9][N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(N(C(C)C)C(C)C)C.O.ON1C2C=CC=CC=2N=N1.F[B-](F)(F)F.N1(OC(N(C)C)=[N+](C)C)C2C=CC=CC=2N=N1.[C:62]([C:66]1[CH:72]=[CH:71][C:69]([NH2:70])=[CH:68][CH:67]=1)([CH3:65])([CH3:64])[CH3:63]>C1COCC1>[C:62]([C:66]1[CH:67]=[CH:68][C:69]([NH:70][C:17]([CH:14]2[CH2:15][CH2:16][C:10]3([O:9][N:8]=[C:7]([C:1]4[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=4)[CH2:11]3)[CH2:12][CH2:13]2)=[O:19])=[CH:71][CH:72]=1)([CH3:65])([CH3:63])[CH3:64]
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 5

HCID 698614-Tert-ButylanilineHCID 81531DiisopropylethylamineHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 27960291-Hydroxybenzotriazole hydrateHCID 579514503-Phenyl-1-oxa-2-azaspiro[4.5]dec-2-ene-8-carboxylic acid

生成物 1

HCID 57951455
3-Phenyl-1-oxa-2-azaspiro[4.5]dec-2-ene-8-carboxylic acid-(4-tert-butylphenyl)amide

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

3-Phenyl-1-oxa-2-azaspiro[4.5]dec-2-ene-8-carboxylic acid (400 mg, 1.5 mmol) was slowly added to a solution of N-ethyldiisopropylamine (662 mg, 4.6 mmol), 1-hydroxybenzotriazole hydrate (206 mg, 1.5 mmol), O-(benzotriazol-1-yl)-N,N,N′,N′-tetramethyluronium tetrafluoroborate (496 mg, 1.5 mmol) and 4-tert-butylaniline (230 mg, 1.5 mmol) in abs. THF (11 ml). The reaction mixture was stirred overnight and the solvent removed under vacuum. The residue was taken up in EtOAc (75 ml). The organic phase was washed successively with sat. aq. NaCl solution, sat. aq. NaHCO3 solution, sat. aq. ammonium sulphate solution and sat. aq. NaCl solution, dried over magnesium sulphate and the solvent removed under vacuum. The desired product 3-phenyl-1-oxa-2-azaspiro[4.5]dec-2-ene-8-carboxylic acid-(4-tert-butylphenyl)amide was obtained as a diastereomer mixture in a yield of 220 mg (37% of the theoretical amount).

後処理

  1. customthe solvent removed under vacuum
  2. washThe organic phase was washed successively with sat. aq. NaCl solution, sat. aq. NaHCO3 solution, sat. aq. ammonium sulphate solution and sat. aq. NaCl solution
  3. dry with materialdried over magnesium sulphate
  4. customthe solvent removed under vacuum

出典と根拠

ORDレコード
ord-46c67fa089eb4a6e99cc3074f495f765
出典データセット
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07981883B2

反応ノート

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