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o-Fluorobenzaldehyde → HCID 22064650, 화합물

HRID 1828111
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HRID 1828111 반응식
[NH2:1][C:2]1[CH:27]=[C:26]([C:28]#[N:29])[CH:25]=[CH:24][C:3]=1[CH2:4][NH:5][C:6](=[O:23])[CH:7]([O:20][CH2:21][CH3:22])[N:8]1[C:16](=[O:17])[C:15]2[C:10](=[CH:11][CH:12]=[CH:13][C:14]=2[F:18])[C:9]1=[O:19].[F:30][C:31]1[CH:38]=[CH:37][CH:36]=[CH:35][C:32]=1[CH:33]=O.[BH3-]C#N.[Na+]>CO.[Cl-].[Cl-].[Zn+2]>[C:28]([C:26]1[CH:25]=[CH:24][C:3]([CH2:4][NH:5][C:6](=[O:23])[CH:7]([O:20][CH2:21][CH3:22])[N:8]2[C:16](=[O:17])[C:15]3[C:10](=[CH:11][CH:12]=[CH:13][C:14]=3[F:18])[C:9]2=[O:19])=[C:2]([NH:1][CH2:33][C:32]2[CH:35]=[CH:36][CH:37]=[CH:38][C:31]=2[F:30])[CH:27]=1)#[N:29]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 67970o-FluorobenzaldehydeHCID 5003444Sodium cyanoborohydrideHCID 22064712HCID 22064712, 화합물

생성물 1

HCID 22064650HCID 22064650, 화합물수율 76%

시약·촉매·용매 2

HCID 3007855Zincchloride촉매HCID 887Methanol용매2회

실험 절차

(RS)-N-(2-amino-4-cyano-benzyl)-2-ethoxy-2-(4-fluoro-1,3-dioxo-1,3-dihydro-isoindol-2-yl)-acetamide (0.060 g) was treated in MeOH (1 ml) successively with 2-fluoro-benzaldehyde (56 mg) and 1 ml of a MeOH-solution containing scrupulously dried ZnCl2 (83 mg) and NaCNBH3 (29 mg). The reaction mixture was stirred for 6 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=6/4) to yield (RS)-N-[4-cyano-2-(2-fluoro-benzylamino)-benzyl ]-2-ethoxy-2-(4-fluoro-1,3-dioxo-1,3-dihydro-isoindol-2-yl)-acetamide (58 mg) as yellow oil, MS 505.4 ([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=6/4)

출처 및 근거

ORD 기록
ord-db8aa210a3b24b2eb7e2548c1e2f2400
출처 데이터셋
uspto-grants-2006_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07056932B2

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