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1,1-Dichloroethane → HCID 178479173, 화합물

HRID 849410
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HRID 849410 반응식
[C:1]([C:3]1[CH:4]=[CH:5][C:6]2[NH:12][CH2:11][C@@H:10]([CH2:13][C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[N:9]([C:20](=[O:28])[CH2:21][C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[CH2:8][C:7]=2[CH:29]=1)#[N:2].[CH:30]([C:32]1[N:33]=[CH:34][NH:35][CH:36]=1)=O.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].[Cl:51]C(Cl)C>CC(O)=O.C(Cl)(Cl)Cl.[NH4+].[OH-].C([O-])(O)=O.[Na+]>[ClH:51].[C:1]([C:3]1[CH:4]=[CH:5][C:6]2[N:12]([CH2:30][C:32]3[N:33]=[CH:34][NH:35][CH:36]=3)[CH2:11][C@@H:10]([CH2:13][C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[N:9]([C:20](=[O:28])[CH2:21][C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[CH2:8][C:7]=2[CH:29]=1)#[N:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 4

HCID 63651,1-DichloroethaneHCID 764281H-Imidazole-4-carbaldehydeHCID 5049666Sodium triacetoxyborohydride2회HCID 53636257(R)-7-cyano-2,3,4,5-tetrahydro-4-(phenylacetyl)-3-(phenylmethyl)-1H-1,4-benzodiazepine2회

생성물 1

HCID 178479173HCID 178479173, 화합물

시약·촉매·용매 4

HCID 176
Acetic Acid
용매
HCID 6212Chloroform용매
HCID 14923Ammonium Hydroxide용매
HCID 516892Sodium Bicarbonate용매

실험 절차

To a refluxing solution of (R)-7-cyano-2,3,4,5-tetrahydro-4-(phenylacetyl)-3-(phenylmethyl)-1H-1,4-benzodiazepine (prepared from Compound C of Example 248 by EDC/HOAt coupling with phenylacetic acid, 0.100 g, 0.26 mmol) and 4-formylimidazole (0.025 g, 0.26 mmol) in AcOH (0.3 mL) and dichloroethane (0.5 mL) with 3 A sieves was added sodium triacetoxyborohydride (0.055 g, 0.26 mmol). The mixture was stirred 16 hr, and then for 3 days, with additional aldehyde and sodium triacetoxyborohydride (3×1 eq each) added each day. The mixture was diluted with CHCl3 (10 mL), NH4OH (5 mL) and NaHCO3 (5 mL), and stirred for 30 min. The layers were separated and the aqueous layer was extracted with CHCl3 (2×20 mL). The combined organic extracts were washed with NaHCO3, water and brine, dried over MgSO4, filtered and concentrated. The product was purified by preparative HPLC (gradient of 20-90% aqueous methanol with 1% TFA) and the HCl salt formed to afford Example 300 as a light yellow solid (4 mg, 3%). MS (M+H)+ =462+

후처리

  1. waitfor 3 days
  2. stirringstirred for 30 min
  3. customThe layers were separated
  4. extractionthe aqueous layer was extracted with CHCl3 (2×20 mL)
  5. washThe combined organic extracts were washed with NaHCO3, water and brine
  6. dry with materialdried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customThe product was purified by preparative HPLC (gradient of 20-90% aqueous methanol with 1% TFA)

출처 및 근거

ORD 기록
ord-8d58fb358b114384943d818760f94b02
출처 데이터셋
uspto-grants-2000_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06011029

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