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Acetic Acid → 1-(5,7,8,9-Tetrahydro-1H-spiro[cyclohepta[f]indazole-6,2'-[1,3]dioxolan]-1-yl)ethanone

HRID 718815
ノート
印刷プレビュー

反応式

HRID 718815 の反応式
[CH3:1][C:2]1[C:16]([NH:17][C:18](=[O:20])[CH3:19])=[CH:15][C:5]2[CH2:6][CH2:7][CH2:8][C:9]3([CH2:14][C:4]=2[CH:3]=1)[O:13][CH2:12][CH2:11][O:10]3.CC([O-])=O.[K+].CC(O)=O.C(OC(=O)C)(=O)C.C1OCCOCCOCCOCCOCCOC1.C(O[N:61]=O)CC(C)C.C([O-])(O)=O.[Na+]>FC1C=CC(N2C3C(=CC=C(CCCC(O)=O)C=3)C=N2)=CC=1.C(Cl)(Cl)Cl>[O:10]1[CH2:11][CH2:12][O:13][C:9]21[CH2:14][C:4]1[CH:3]=[C:2]3[C:16](=[CH:15][C:5]=1[CH2:6][CH2:7][CH2:8]2)[N:17]([C:18](=[O:20])[CH3:19])[N:61]=[CH:1]3
参加物実験手順後処理出典と根拠反応ノート

参加物

10

反応物 7

HCID 176Acetic AcidHCID 7918Acetic Anhydride2 回HCID 8053Isoamyl Nitrite2 回HCID 2855718-Crown-6HCID 516892Sodium Bicarbonate2 回HCID 517044Potassium AcetateHCID 86722424N-(3-Methyl-5,7,8,9-tetrahydrospiro[benzo[7]annulene-6,2'-[1,3]dioxolan]-2-yl)acetamide

生成物 1

HCID 867224251-(5,7,8,9-Tetrahydro-1H-spiro[cyclohepta[f]indazole-6,2'-[1,3]dioxolan]-1-yl)ethanone収率 48.1%

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒HCID 867223224-(1-(4-fluorophenyl)-1H-indazol-6-yl)butanoic acid溶媒

実験手順

In a 20 L 3 necked flask, N-(3-Methyl-5,7,8,9-tetrahydrospiro[benzo[7]annulene-6,2′-[1,3]dioxolan]-2-yl)acetamide (78) (900 g, 3.27 mol) was dissolved in chloroform (10 L). KOAc (634 g, 6.54 mol), HOAc (382 mL, 6.54 mol), acetic anhydride (655 mL, 6.54 mol), 18-crown-6 (130 g, 523 mmol) and isoamylnitrite (1.30 L, 13.4 mol) were respectively added. The mixture was heated to reflux for about 3 h. Acetic anhydride (900 mL, 9.54 mol) and isoamylnitrite (1.80 L, 13.4 mol) were added and the mixture was heated to reflux overnight. The reaction mixture was cooled to rt and then carefully poured into sat. aq. NaHCO3 (80 L). The pH was carefully adjusted to basic with NaHCO3. The layers were separated and the aq. phase was extracted with DCM (2×15 L). The combined organic layers were concentrated under reduced pressure. tert-Butyl methyl ether (1500 mL) was added and the resulting slurry was stirred for about 1 h. The precipitate was collected by filtration to afford 1-(5,7,8,9-tetrahydro-1H-spiro[cyclohepta[f]indazole-6,2′-[1,3]dioxolan]-1-yl)ethanone (79) (450 g, 48% yield) as a yellow solid. 1H NMR (300 MHz, DMSO): δ 8.38 (s, 1H), 8.05 (s, 1H), 7.72 (s, 1H), 3.95 (m, 2H), 3.82 (m, 2H), 3.16 (s, 2H), 2.96 (m, 2H), 2.64 (s, 3H), 1.84 (m, 2H), 1.62 (m, 2H).

後処理

  1. temperatureThe mixture was heated
  2. temperatureto reflux for about 3 h
  3. temperaturethe mixture was heated
  4. temperatureto reflux overnight
  5. customThe layers were separated
  6. extractionthe aq. phase was extracted with DCM (2×15 L)
  7. concentrationThe combined organic layers were concentrated under reduced pressure
  8. additiontert-Butyl methyl ether (1500 mL) was added
  9. filtrationThe precipitate was collected by filtration

出典と根拠

ORDレコード
ord-5df592074e2a41ed9edfa7535d8a94b4
出典データセット
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09193744B2

反応ノート

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