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Hydrochloric Acid → 4-(2,4-Dioxo-8-oxa-1,3-diazaspiro[4.5]decan-3-yl)-2-(trifluoromethyl)-benzonitrile

HRID 725209
ノート
印刷プレビュー

反応式

HRID 725209 の反応式
N=[C:2]1[C:6]2([CH2:11][CH2:10][O:9][CH2:8][CH2:7]2)[NH:5][C:4](=[O:12])[N:3]1[C:13]1[CH:20]=[CH:19][C:16]([C:17]#[N:18])=[C:15]([C:21]([F:24])([F:23])[F:22])[CH:14]=1.C[OH:26].C(Cl)(Cl)Cl.Cl>O>[O:12]=[C:4]1[N:3]([C:13]2[CH:20]=[CH:19][C:16]([C:17]#[N:18])=[C:15]([C:21]([F:24])([F:22])[F:23])[CH:14]=2)[C:2](=[O:26])[C:6]2([CH2:7][CH2:8][O:9][CH2:10][CH2:11]2)[NH:5]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 6212ChloroformHCID 153454974-(4-Imino-2-oxo-8-oxa-1,3-diazaspiro[4.5]decan-3-yl)-2-(trifluoromethyl)-benzonitrile

生成物 1

HCID 153454984-(2,4-Dioxo-8-oxa-1,3-diazaspiro[4.5]decan-3-yl)-2-(trifluoromethyl)-benzonitrile

試薬・触媒・溶媒 1

HCID 962
Water
溶媒

実験手順

1.66 g of the product of Example 1 were introduced into 30 ml of methanol, 10 ml of chloroform and 10 ml of 2N hydrochloric acid, and the mixture was refluxed for 50 minutes. 100 ml of water were added and extraction was carried out 3 times with ethyl acetate. The organic phase was washed with salt water, dried and purified on silica with methylene chloride-acetone: 85-15 as eluant. The resultant product was dissolved in 100 ml of isopropanol at about 70° C. and filtration was carried out, followed by concentrating, ice-cooling for one hour, separating and drying to obtain 1.425 g of the expected product (white crystals) melting at 192°-193° C.

後処理

  1. temperaturethe mixture was refluxed for 50 minutes
  2. extractionextraction
  3. washThe organic phase was washed with salt water
  4. customdried
  5. custompurified on silica with methylene chloride-acetone
  6. dissolutionThe resultant product was dissolved in 100 ml of isopropanol at about 70° C.
  7. filtrationfiltration
  8. concentrationby concentrating
  9. temperatureice-cooling for one hour
  10. customseparating
  11. customdrying

出典と根拠

ORDレコード
ord-8d98e15db380498cb2dd1a61b75f3775
出典データセット
uspto-grants-1998_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05705654

反応ノート

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