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Ammonium Chloride → HCID 19364897、化合物

HRID 850798
ノート
印刷プレビュー

反応式

HRID 850798 の反応式
[C:1]([C:9]1[C:10](=[O:25])[C:11]2[CH:12]=[CH:13][CH:14]=[C:15]3[C:23]=2[N:22]([CH:24]=1)[C:21]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]3=1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Cl-].[NH4+]>O1CCCC1>[OH:8][CH:1]([C:9]1[C:10](=[O:25])[C:11]2[CH:12]=[CH:13][CH:14]=[C:15]3[C:23]=2[N:22]([CH:24]=1)[C:21]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]3=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 25517Ammonium ChlorideHCID 21252825HCID 21252825、化合物

生成物 1

HCID 19364897HCID 19364897、化合物収率 44%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

5-benzoyl-4H-pyrido[3,2,1-jk]carbazole-4-one (80 mg) produced in Example 145 was dissolved in anhydrous tetrahydrofuran (80 ml), and lithium aluminium tri-t-butoxyhydride (76 mg) was added to the solution in an ice bath, and the mixture was stirred for 30 minutes. Saturated aqueous solution of ammonium chloride of an adequate amount was added to the reaction mixture, and the mixture was heated to room temperature, and extracted with ethyl acetate. The ethyl acetate layer was washed with saturated aqueous solution of sodium chloride, and dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residual crude crystals were re-precipitated from hexane and ethyl acetate to obtain the title compound (35 mg, 44%).

後処理

  1. extractionextracted with ethyl acetate
  2. washThe ethyl acetate layer was washed with saturated aqueous solution of sodium chloride
  3. dry with materialdried over anhydrous sodium sulfate
  4. customthe solvent was evaporated under reduced pressure
  5. customThe residual crude crystals were re-precipitated from hexane and ethyl acetate

出典と根拠

ORDレコード
ord-217c9e6c60ed4495ad904d83d029b179
出典データセット
uspto-grants-2000_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06018046

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート