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Sodium borohydride → HCID 67854747, 화합물

HRID 257088
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HRID 257088 반응식
[C:1]([OH:8])(=[O:7])/[CH:2]=[CH:3]/[C:4]([OH:6])=[O:5].[C:9]([C:12]1[CH:17]=[CH:16][C:15]([N:18]2[CH2:23][CH2:22][CH:21]([N:24]([CH3:33])[CH2:25][CH2:26][C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=3)[CH2:20][CH2:19]2)=[CH:14][CH:13]=1)(=[O:11])[CH3:10].[BH4-].[Na+]>CO>[C:1]([OH:8])(=[O:7])/[CH:2]=[CH:3]/[C:4]([OH:6])=[O:5].[C:1]([OH:8])(=[O:7])/[CH:2]=[CH:3]/[C:4]([OH:6])=[O:5].[OH:11][CH:9]([C:12]1[CH:13]=[CH:14][C:15]([N:18]2[CH2:19][CH2:20][CH:21]([N:24]([CH3:33])[CH2:25][CH2:26][C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=3)[CH2:22][CH2:23]2)=[CH:16][CH:17]=1)[CH3:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 4311764Sodium borohydrideHCID 19784367HCID 19784367, 화합물

생성물 1

HCID 67854747HCID 67854747, 화합물수율 18%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

10.4 g (0.32 mol) of the product from Example 12 (as base) were dissolved in 500 ml of methanol and, at 10° C., 18.0 g (0.475 mol) of sodium borohydride were added a little at a time. The mixture was stirred at room temperature for 16 hours and then evaporated in a rotary evaporator. The residue was partitioned between methylene chloride and water, and the organic phase was dried and evaporated in a rotary evaporator. The resulting oil was crystallized as the fumarate. 16.4 g of 1-(4-(1-hydroxyethyl)phenyl)-4-(N-methyl-N-(2-phenylethyl)amino)piperidine difumarate were obtained. Melting point 124°-129° C.

후처리

  1. customevaporated in a rotary evaporator
  2. customThe residue was partitioned between methylene chloride and water
  3. customthe organic phase was dried
  4. customevaporated in a rotary evaporator
  5. customThe resulting oil was crystallized as the fumarate

출처 및 근거

ORD 기록
ord-1f9a38b58c594237870a9d38d237eb2d
출처 데이터셋
uspto-grants-1993_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05260318

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