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Iodoethane → HCID 69018701、化合物

HRID 1437918
ノート
印刷プレビュー

反応式

HRID 1437918 の反応式
I[CH2:2][CH3:3].[Cl:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[N:11]1[C:19](=[O:20])[C:18]2[C@@H:17]3[C:21]([CH3:23])([CH3:22])[C@@:14]([CH3:24])([CH2:15][CH2:16]3)[C:13]=2[NH:12]1.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O.C(OCC)(=O)C>[Cl:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[N:11]1[C:19]([O:20][CH2:2][CH3:3])=[C:18]2[C:13]([C:14]3([CH3:24])[C:21]([CH3:23])([CH3:22])[CH:17]2[CH2:16][CH2:15]3)=[N:12]1.[Cl:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[N:11]1[C:19](=[O:20])[C:18]2[C@@H:17]3[C:21]([CH3:23])([CH3:22])[C@@:14]([CH3:24])([CH2:15][CH2:16]3)[C:13]=2[N:12]1[CH2:2][CH3:3]
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 3

HCID 6340IodoethaneHCID 11430Potassium CarbonateHCID 57941362HCID 57941362、化合物2 回

生成物 2

HCID 57941485HCID 57941485、化合物収率 9%HCID 69018701HCID 69018701、化合物収率 16%

試薬・触媒・溶媒 2

HCID 6228
Dimethylformamide
溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

Iodoethane (14 μL, 0.18 mmol) was added to (4S,7R)-2-(2-chloro-phenyl)-7,8,8-trimethyl-1,2,4,5,6,7-hexahydro-4,7-methano-indazol-3-one (Intermediate 10; 47 mg, 0.16 mmol) and potassium carbonate (43 mg, 0.31 mmol) in dimethylformamide (1 mL). The mixture was heated at 60 degrees for 4 h, and then stirred at room temperature over the weekend. The reaction mixture was diluted with ethyl acetate and washed with NaOH. The solvent was evaporated from the ethyl acetate layer and the residue was purified by flash chromatography, eluting with 0-70% ethyl acetate/hexanes, to give 2-(2-chloro-phenyl)-3-ethoxy-7,8,8-trimethyl-4,5,6,7-tetrahydro-2H-4,7-methano-indazole (12.3 mg, 16%) and (4S,7R)-2-(2-chloro-phenyl)-1-ethyl-7,8,8-trimethyl-1,2,4,5,6,7-hexahydro-4,7-methano-indazol-3-one (4.4 mg, 9%). APCI-MS (M+H) 331.

後処理

  1. temperatureThe mixture was heated at 60 degrees for 4 h
  2. washwashed with NaOH
  3. customThe solvent was evaporated from the ethyl acetate layer
  4. customthe residue was purified by flash chromatography
  5. washeluting with 0-70% ethyl acetate/hexanes

出典と根拠

ORDレコード
ord-c57f712bcfe3441383c43008e880fdf5
出典データセット
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07622492B2

反応ノート

読み込み中…

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