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o-Fluorobenzaldehyde → HCID 22064641, 화합물

HRID 1828106
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HRID 1828106 반응식
[NH2:1][C:2]1[CH:26]=[C:25]([C:27]#[N:28])[CH:24]=[CH:23][C:3]=1[CH2:4][NH:5][C:6](=[O:22])[CH:7]([O:19][CH2:20][CH3:21])[N:8]1[CH2:16][C:15]2[C:10](=[CH:11][CH:12]=[CH:13][C:14]=2[CH3:17])[C:9]1=[O:18].[F:29][C:30]1[CH:37]=[CH:36][CH:35]=[CH:34][C:31]=1[CH:32]=O.[BH3-]C#N.[Na+]>CO.[Cl-].[Cl-].[Zn+2]>[C:27]([C:25]1[CH:24]=[CH:23][C:3]([CH2:4][NH:5][C:6](=[O:22])[CH:7]([O:19][CH2:20][CH3:21])[N:8]2[CH2:16][C:15]3[C:10](=[CH:11][CH:12]=[CH:13][C:14]=3[CH3:17])[C:9]2=[O:18])=[C:2]([NH:1][CH2:32][C:31]2[CH:34]=[CH:35][CH:36]=[CH:37][C:30]=2[F:29])[CH:26]=1)#[N:28]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 67970o-FluorobenzaldehydeHCID 5003444Sodium cyanoborohydrideHCID 22064672HCID 22064672, 화합물

생성물 1

HCID 22064641HCID 22064641, 화합물수율 85.5%

시약·촉매·용매 2

HCID 3007855Zincchloride촉매HCID 887Methanol용매2회

실험 절차

(RS)-N-(2-Amino-4-cyano-benzyl)-2-ethoxy-2-(4-methyl-1-oxo-1,3-dihydro-isoindol-2-yl)-acetamide (0.101 g) was treated in MeOH (2 ml) successively with 2-fluoro-benzaldehyde (99 mg) and 1 ml of a MeOH-solution containing scrupulously dried ZnCl2 (145 mg) and NaCNBH3 (50 mg). The reaction mixture was stirred for 16 h at 50–55° C., poured onto crashed ice and extracted two times with ethyl acetate. The combined organic layers were washed with water and brine and dried over magnesium sulfate. The solvent was removed under reduced pressure and the residue purified by column chromatography (silica gel, hexane/AcOEt=1/1) to give (RS)-N-[4-cyano-2-(2-fluoro-benzylamino)-benzyl]-2-ethoxy-2-(4-methyl-1-oxo-1,3-dihydro-isoindol-2-yl)-acetamide (111 mg) as colorless oil, MS 487.4 ([M+H]+).

후처리

  1. additionpoured
  2. extractionextracted two times with ethyl acetate
  3. washThe combined organic layers were washed with water and brine
  4. dry with materialdried over magnesium sulfate
  5. customThe solvent was removed under reduced pressure
  6. customthe residue purified by column chromatography (silica gel, hexane/AcOEt=1/1)

출처 및 근거

ORD 기록
ord-29d7f66a5b1d485eae0cd00143051d4d
출처 데이터셋
uspto-grants-2006_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07056932B2

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