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2-(Dimethylamino)acetohydrazide → HCID 178483332、化合物

HRID 1273020
ノート
印刷プレビュー

反応式

HRID 1273020 の反応式
O1C2C=CC=CC=2C=C1[C:10]1[C:18]2[C:13](=[CH:14][CH:15]=[C:16]([C:19]#[N:20])[CH:17]=2)[N:12]([CH:21]2[CH2:26][CH2:25][CH2:24][CH2:23][O:22]2)[N:11]=1.[NH2:27][NH:28][C:29](=O)[CH2:30][N:31]([CH3:33])[CH3:32].[CH3:35][O-:36].[Na+]>CO.ClCCl>[O:36]1[C:15]2[CH:14]=[CH:13][CH:18]=[CH:17][C:16]=2[CH:19]=[C:35]1[CH:26]1[CH2:25][CH2:24][CH2:23][O:22][CH:21]1[N:12]1[C:13]2[C:18](=[CH:17][C:16]([C:19]3[NH:27][N:28]=[C:29]([CH2:30][N:31]([CH3:33])[CH3:32])[N:20]=3)=[CH:15][CH:14]=2)[CH:10]=[N:11]1
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 3

HCID 683192-(Dimethylamino)acetohydrazide2 回HCID 10942334Sodium MethoxideHCID 224798583-benzo[b]furan-2-yl-1-perhydro-2H-pyran-2-yl-1H-indazole-5-carbonitrile

生成物 1

HCID 178483332HCID 178483332、化合物収率 7%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒3 回
HCID 6344
Dichloromethane
溶媒

反応条件

温度
100 °C

実験手順

To a suspension of 3-benzo[d]furan-2-yl-1-perhydro-2H-pyran-2-yl-1H-indazole-5-carbonitrile (167 mg, 0.49 mmol) and N-amino-2-(dimethylamino)acetamide (171 mg, 1.46 mmol) in anhydrous methanol (1.0 mL) in a screw-top pressure tube was added sodium methoxide (445 μL of a 25% w/w in methanol). The tube was sealed and heated in a 100° C. oil bath for 21 h. An additional amount of N-amino-2-(dimethylamino)acetamide (171 mg, 1.46 mmol) was added and the reaction heated for an additional 2 days. The reaction was cooled, evaporated to dryness and partitioned between ethyl acetate and satd. ammonium chloride. The organic layer was separated, washed with brine, dried over MgSO4 and concentrated in vacuo to give a yellow solid. Purification of the residue by flash chromatography on silica gel using 5% methanol in dichloromethane then 20% methanol in dichloromethane gave the desired product (15 mg, 7% yield) as a pale yellow foam. ES-MS (m/z) 443 [M+H]+.

後処理

  1. customThe tube was sealed
  2. temperaturethe reaction heated for an additional 2 days
  3. temperatureThe reaction was cooled
  4. customevaporated to dryness
  5. custompartitioned between ethyl acetate and satd
  6. customThe organic layer was separated
  7. washwashed with brine
  8. dry with materialdried over MgSO4
  9. concentrationconcentrated in vacuo
  10. customto give a yellow solid
  11. customPurification of the residue by flash chromatography on silica gel using 5% methanol in dichloromethane

出典と根拠

ORDレコード
ord-43d308c361124e3089d5bdfd9d64dfbd
出典データセット
uspto-grants-2007_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07208513B2

反応ノート

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