Sodium borohydride → 1-(7-Chloro-6-methyl-2,3,4,5-tetrahydro-1,4-benzoxazepin-9-yl)ethanol

HRID 626817노트

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HRID 626817 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([C:14](=[O:16])[CH3:15])[C:5]2[O:11][CH2:10][CH2:9][N:8]=[CH:7][C:6]=2[C:12]=1[CH3:13].[BH4-].[Na+]>CO>[Cl:1][C:2]1[CH:3]=[C:4]([CH:14]([OH:16])[CH3:15])[C:5]2[O:11][CH2:10][CH2:9][NH:8][CH2:7][C:6]=2[C:12]=1[CH3:13]

참가 물질

4

반응물 2

HCID 4311764Sodium borohydrideHCID 866975131-(7-Chloro-6-methyl-2,3-dihydro-1,4-benzoxazepin-9-yl)ethanone

생성물 1

HCID 866975141-(7-Chloro-6-methyl-2,3,4,5-tetrahydro-1,4-benzoxazepin-9-yl)ethanol수율 92.3%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
0 °C

실험 절차

1-(7-Chloro-6-methyl-2,3-dihydro-1,4-benzoxazepin-9-yl)ethanone (630 mg, 2.6 mmol) was stirred in methanol (20 mL) and cooled to 0° C. Sodium tetrahydroborate (150 mg, 4.0 mmol) was added. The mixture was stirred for 1 hour at room temperature and evaporated. The mixture was extracted with ethyl acetate, washed with saturated sodium bicarbonate, brine, dried over sodium sulfate, filtered and evaporated gave the desired compound (580 mg, 90%). LCMS calculated for C12H17ClNO2 (M+H)+: m/z=242.1; found: 242.0.

후처리

  1. customevaporated
  2. extractionThe mixture was extracted with ethyl acetate
  3. washwashed with saturated sodium bicarbonate, brine
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. customevaporated

출처 및 근거

ORD 기록
ord-c576c389c45d4d34924bfe5aec4b848e
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09309251B2

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