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Sodium hydride → HCID 53855886, 화합물

HRID 865925
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HRID 865925 반응식
[H-].[Na+].[CH3:3][C:4]1[C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=2[NH:8][C:7](=[O:15])[CH:6]([NH:16][C:17](=[O:26])[O:18][CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[N:5]=1.Br[CH2:28][C:29]([N:31]([CH3:38])[C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1)=[O:30]>CN(C=O)C>[CH3:3][C:4]1[C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=2[N:8]([CH2:28][C:29]([N:31]([CH3:38])[C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)=[O:30])[C:7](=[O:15])[CH:6]([NH:16][C:17](=[O:26])[O:18][CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[N:5]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 344952-Bromo-N-methyl-N-phenylacetamideHCID 135744107HCID 135744107, 화합물

생성물 1

HCID 53855886HCID 53855886, 화합물수율 39%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

80% Sodium hydride in oil (102 mg) was added to a solution of phenylmethyl [2,3-dihydro-5-methyl-2-oxo-1H-1,4-benzodiazepin-3-yl]carbamate (1.00 g) in dry DMF (10 ml) under nitrogen. The mixture was stirred for 0.5 h at 23° and was treated with a solution of 2-bromo-N-methyl-N-phenylacetamide (707 mg) in dry DMF (1 ml). The mixture was stirred at 23° for 1 h, partitioned between phosphate buffer solution (pH6.5) and EA, the organic phase was washed with water and dried. The solvent was evaporated in vacuo and the residue was purified by chromatography on alumina. Elution with MeOH-DCM (1:50) gave the title compound (568 mg).

후처리

  1. stirringThe mixture was stirred at 23° for 1 h
  2. custompartitioned between phosphate buffer solution (pH6.5) and EA
  3. washthe organic phase was washed with water
  4. customdried
  5. customThe solvent was evaporated in vacuo
  6. customthe residue was purified by chromatography on alumina
  7. washElution with MeOH-DCM (1:50)

출처 및 근거

ORD 기록
ord-df6a8fce052d47c18f89938a28d045c4
출처 데이터셋
uspto-grants-1996_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05569654

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