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Lithium Hydroxide → HCID 22632528, 화합물

HRID 2417541
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HRID 2417541 반응식
[Cl:1][C:2]1[CH:32]=[CH:31][C:5]([C:6]([N:8]2[CH2:14][C:13]3[CH:15]=[CH:16][CH:17]=[CH:18][C:12]=3[N:11]([CH2:19][C:20]3[CH:25]=[CH:24][CH:23]=[C:22]([C:26](OC)=O)[CH:21]=3)[C:10](=[O:30])[CH2:9]2)=[O:7])=[CH:4][CH:3]=1.[OH-].[Li+].[Cl:35]C(OCC)=O.[BH4-].[Na+].CS(Cl)(=O)=O>C1COCC1.ClCCl.C(OCC)(=O)C.C(N(CC)CC)C>[Cl:1][C:2]1[CH:32]=[CH:31][C:5]([C:6]([N:8]2[CH2:14][C:13]3[CH:15]=[CH:16][CH:17]=[CH:18][C:12]=3[N:11]([CH2:19][C:20]3[CH:25]=[CH:24][CH:23]=[C:22]([CH2:26][Cl:35])[CH:21]=3)[C:10](=[O:30])[CH2:9]2)=[O:7])=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

10

반응물 5

HCID 3939Lithium HydroxideHCID 10928Ethyl chloroformateHCID 31297Methanesulfonyl chlorideHCID 4311764Sodium borohydrideHCID 22632602HCID 22632602, 화합물

생성물 1

HCID 22632528HCID 22632528, 화합물

시약·촉매·용매 4

HCID 6344
Dichloromethane
용매
HCID 8028Tetrahydrofuran용매2회
HCID 8471Triethylamine용매2회
HCID 8857Ethyl Acetate용매2회

실험 절차

145 mg (0.32 mmol) of 4-(4-chlorobenzoyl)-1-(3-methoxycarbonylbenzyl)-1,3,4,5-tetrahydrobenzo[e][1,4]diazepin-2-on obtained in step 1 was dissolved in 3 ml of THF. 1.6 ml of 1 M aqueous lithium hydroxide solution was added to the obtained solution, and they were stirred overnight. After the treatment with ethyl acetate as the extracting solvent by an ordinary method, the obtained crude product was dissolved in 5 ml of THF. 0.1 ml (0.7 mmol) of triethylamine and 0.05 ml (0.5 mmol) of ethyl chloroformate were added to the obtained solution under cooling with ice, and they were stirred for 30 minutes. A piece of ice and 50 mg (1.4 mmol) of sodium borohydride were added to the obtained mixture. The temperature was elevated to room temperature, and the obtained mixture was stirred overnight. The solvent was evaporated, and the obtained crude product was dissolved in 8 ml of dichloromethane. 0.03 ml (0.22 mmol)) of triethylamine and 0.01 ml (0.13 mmol) of methanesulfonyl chloride were added to the obtained solution under cooling with ice, and they were stirred overnight. After the treatment with ethyl acetate as the extracting solvent by an ordinary method, the crude product was obtained. After the purification by the silica gel column chromatography, the title compound was obtained.

후처리

  1. temperatureunder cooling with ice, and they
  2. stirringwere stirred for 30 minutes
  3. customwas elevated to room temperature
  4. stirringthe obtained mixture was stirred overnight
  5. customThe solvent was evaporated
  6. customthe obtained crude product
  7. temperatureunder cooling with ice, and they
  8. stirringwere stirred overnight
  9. customAfter the purification by the silica gel column chromatography

출처 및 근거

ORD 기록
ord-0c956b5e9c684f29aa812978f6ea970d
출처 데이터셋
uspto-grants-2004_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06825191B2

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