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Sodium borohydride → HCID 13355660、化合物

HRID 1111966
ノート
印刷プレビュー

反応式

HRID 1111966 の反応式
[BH4-].[Na+].[NH2:3][C:4]1[C:9]([C:10]#[N:11])=[CH:8][C:7]([C:12](=[O:18])[CH2:13][NH:14][CH:15]2[CH2:17][CH2:16]2)=[CH:6][C:5]=1[Br:19]>O1CCCC1.O>[NH2:3][C:4]1[C:9]([C:10]#[N:11])=[CH:8][C:7]([CH:12]([OH:18])[CH2:13][NH:14][CH:15]2[CH2:16][CH2:17]2)=[CH:6][C:5]=1[Br:19]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 4311764Sodium borohydrideHCID 13355652HCID 13355652、化合物

生成物 1

HCID 13355660HCID 13355660、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

3 gm of sodium borohydride were added at room temperature to a solution of 7.5 gm of 4'-amino-3'-bromo-5'-cyano-2-cyclopropylamino-acetophenone in 200 ml of tetrahydro-furan and 100 ml of water, and the mixture was stirred for one hour. Thereafter, the excess sodium borohydride was destroyed by addition of acetone. The insoluble part of the mixture was filtered off, and the solvents were distilled out of the filtrate in vacuo. The residue was dissolved in hot isopropanol, and the hydrochloride of 1-(4'-amino-3'-bromo-5'-cyano-phenyl)-2-cyclopropylanino-ethanol was precipitated by addition of isopropanolic hydrochloric acid, and recrystallized from isopropanol. M.p. 190°-193° C. (decomp.).

後処理

  1. customThereafter, the excess sodium borohydride was destroyed by addition of acetone
  2. filtrationThe insoluble part of the mixture was filtered off
  3. distillationthe solvents were distilled out of the filtrate in vacuo
  4. dissolutionThe residue was dissolved in hot isopropanol
  5. customthe hydrochloride of 1-(4'-amino-3'-bromo-5'-cyano-phenyl)-2-cyclopropylanino-ethanol was precipitated by addition of isopropanolic hydrochloric acid
  6. customrecrystallized from isopropanol

出典と根拠

ORDレコード
ord-94fbaf1d7ef84cdeb3fded3c5a8d5493
出典データセット
uspto-grants-1978_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04119710

反応ノート

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