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Hydrochloric Acid → HCID 19973110、化合物

HRID 1451952
ノート
印刷プレビュー

反応式

HRID 1451952 の反応式
O[CH2:2][CH2:3][NH:4][C:5](=[O:25])[C:6]([F:24])([F:23])[C:7]([C:15]1[CH:20]=[CH:19][C:18]([F:21])=[CH:17][C:16]=1[F:22])([OH:14])[CH2:8][N:9]1[CH:13]=[N:12][CH:11]=[N:10]1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.N(C(OCC)=O)=NC(OCC)=O.Cl>O.C(OCC)(=O)C.O1CCCC1>[N:4]1([C:5]([C:6]([F:24])([F:23])[C:7]([C:15]2[CH:20]=[CH:19][C:18]([F:21])=[CH:17][C:16]=2[F:22])([OH:14])[CH2:8][N:9]2[CH:13]=[N:12][CH:11]=[N:10]2)=[O:25])[CH2:3][CH2:2]1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 11776TriphenylphosphineHCID 220568ethyl N-ethoxycarbonyliminocarbamateHCID 19973077HCID 19973077、化合物

生成物 1

HCID 19973110HCID 19973110、化合物収率 38%

試薬・触媒・溶媒 3

HCID 962Water溶媒
HCID 8028
Tetrahydrofuran
溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

To 10 ml of dried tetrahydrofuran were added 0.36 g of N-(2-hydroxyethyl)-3-(2,4-difluorophenyl)-2,2-difluoro-3-hydroxy-4-(1H-1,2,4-triazol-1-yl)butanamide, 0.39 g of triphenylphosphine and 0.26 g of diethyl azodicarboxylate. The resulting mixture was subjected to reaction at 20°-25° C. for 12 hours. The reaction mixture was introduced into a mixed solvent consisting of 20 ml of ethyl acetate and 10 ml of water. The resulting solution was adjusted to pH 2.0 with 6N hydrochloric acid. The organic layer was separated, washed with a saturated aqueous sodium chloride solution, and then dried over anhydrous magnesium sulfate. Thereafter, the solvent was removed by distillation under reduced pressure. The residue thus obtained was purified by a column chromatography (eluant: toluene/ethyl acetate=10/1) to obtain 0.13 g of 1-aziridinylcarbonyl-2-(2,4-difluorophenyl)-1,1-difluoro-2-hydroxy-3-(1H-1,2,4-triazol-1-yl)propane.

後処理

  1. customThe resulting mixture was subjected to reaction at 20°-25° C. for 12 hours
  2. additionThe reaction mixture was introduced into a mixed solvent
  3. customThe organic layer was separated
  4. washwashed with a saturated aqueous sodium chloride solution
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customThereafter, the solvent was removed by distillation under reduced pressure
  7. customThe residue thus obtained
  8. customwas purified by a column chromatography (eluant: toluene/ethyl acetate=10/1)

出典と根拠

ORDレコード
ord-a8bc612a239f4b7085ad6d0ebf161951
出典データセット
uspto-grants-1997_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05605921

反応ノート

読み込み中…

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