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Lithium Hydroxide → HCID 22632528、化合物

HRID 2417541
ノート
印刷プレビュー

反応式

HRID 2417541 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

10

反応物 5

HCID 3939Lithium HydroxideHCID 10928Ethyl chloroformateHCID 31297Methanesulfonyl chlorideHCID 4311764Sodium borohydrideHCID 22632602HCID 22632602、化合物

生成物 1

HCID 22632528HCID 22632528、化合物

試薬・触媒・溶媒 4

HCID 6344
Dichloromethane
溶媒
HCID 8028Tetrahydrofuran溶媒2 回
HCID 8471Triethylamine溶媒2 回
HCID 8857Ethyl Acetate溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-0c956b5e9c684f29aa812978f6ea970d
出典データセット
uspto-grants-2004_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06825191B2

反応ノート

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