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Sodium borohydride → HCID 13355660, 화합물

HRID 1111966
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HRID 1111966 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 4311764Sodium borohydrideHCID 13355652HCID 13355652, 화합물

생성물 1

HCID 13355660HCID 13355660, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

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.).

후처리

  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

출처 및 근거

ORD 기록
ord-94fbaf1d7ef84cdeb3fded3c5a8d5493
출처 데이터셋
uspto-grants-1978_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04119710

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