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Hexane → HCID 19366009、化合物

HRID 850095
ノート
印刷プレビュー

反応式

HRID 850095 の反応式
[CH2:1]([O:3][CH2:4][N:5]1[CH:9]=[N:8][CH:7]=[N:6]1)[CH3:2].C([Li])CCC.CCCCCC.[F:21][C:22]1[CH:27]=[C:26]([F:28])[CH:25]=[CH:24][C:23]=1[C:29]([OH:45])([C:36]([C:38]1[CH:43]=[CH:42][C:41](I)=[CH:40][CH:39]=1)=[CH2:37])[CH2:30][N:31]1[CH:35]=[N:34][CH:33]=[N:32]1.[Na+].[Na+].C(N(CC(O)=O)CC(O)=O)CN(CC([O-])=O)CC([O-])=O.C(=O)([O-])[O-].[Na+].[Na+]>O1CCCC1.[Cl-].[Zn+2].[Cl-].C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[F:21][C:22]1[CH:27]=[C:26]([F:28])[CH:25]=[CH:24][C:23]=1[C:29]([OH:45])([C:36]([C:38]1[CH:43]=[CH:42][C:41]([C:9]2[N:5]([CH2:4][O:3][CH2:1][CH3:2])[N:6]=[CH:7][N:8]=2)=[CH:40][CH:39]=1)=[CH2:37])[CH2:30][N:31]1[CH:35]=[N:34][CH:33]=[N:32]1
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 6

HCID 8058HexaneHCID 10340Sodium CarbonateHCID 3823094HCID 3823094、化合物HCID 13020083Ethylenediaminetetraacetic acid disodium saltHCID 17892901HCID 17892901、化合物HCID 178418339Butyllithium

生成物 1

HCID 19366009
HCID 19366009、化合物
収率 81%

試薬・触媒・溶媒 3

HCID 3007855Zincchloride触媒HCID 178418397HCID 178418397、化合物触媒HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of 1-ethoxymethyl-1,2,4-triazole (0.79 g, 6.2 mmol-see Preparation 27) in tetrahydrofuran (THF) (8 ml) was stirred under a nitrogen atmosphere at -70° C. before treatment with a solution of n-butyllithium in hexane (2.5M, 2.5 ml, 6.2 mmol) The mixture was stirred for 0.25 hours and treated with a solution of anhydrous zinc chloride (1.2 g, 9.3 mmol) in THF (8 ml), then was allowed to warm to room temperature. To this mixture was added tetrakis(triphenylphosphine)palladium (0) (0.06 g, 0.06 mmol) and 2-(2,4-difluorophenyl)-3-(4-iodophenyl)-1-(1,2,4-triazol-1-yl)-3-buten-2-ol (0.7 g, 1.5 mmol-see Preparation 20) and the mixture was heated under reflux for 4 hours. After being cooled, a suspension of ethylenediaminetetraacetic acid disodium salt (10 g, 27 mmol) was added, the mixture was adjusted to pH8 with saturated sodium carbonate solution and extracted with dichloromethane (2×100 ml). The combined extracts were dried (MgSO4) and evaporated under reduced pressure. The residue was chromatographed on silica by gradient elution with dichloromethanelmethanol (98:2, 97:3, 95:5). Fractions containing the desired product were combined, evaporated under reduced pressure and the residue was triturated with ether to afford the title compound (0.55 g, 78%) as a colourless solid, m.p. 160-162° C.

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 4 hours
  3. temperatureAfter being cooled
  4. additionwas added
  5. extractionextracted with dichloromethane (2×100 ml)
  6. dry with materialThe combined extracts were dried (MgSO4)
  7. customevaporated under reduced pressure
  8. customThe residue was chromatographed on silica by gradient elution with dichloromethanelmethanol (98:2, 97:3, 95:5)
  9. additionFractions containing the desired product
  10. customevaporated under reduced pressure
  11. customthe residue was triturated with ether

出典と根拠

ORDレコード
ord-add1f348b890448483ac851a5720fc76
出典データセット
uspto-grants-2000_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06015825

反応ノート

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