Benzoyl chloride → HCID 58054120, 화합물

HRID 75124노트

반응식

HRID 75124 반응식
[N:1]1([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH2:7][CH2:6][CH:5]([C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9])[NH:4][CH2:3][CH2:2]1.[C:22](Cl)(=[O:29])[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1>C(Cl)Cl>[C:22]([N:4]1[CH:5]([C:8]([O:10][C:11]([CH3:13])([CH3:14])[CH3:12])=[O:9])[CH2:6][CH2:7][N:1]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH2:2][CH2:3]1)(=[O:29])[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1

참가 물질

4

반응물 2

HCID 7412Benzoyl chlorideHCID 66660434Di-tert-butyl 1,4-diazepane-1,5-dicarboxylate

생성물 1

HCID 58054120HCID 58054120, 화합물수율 49%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of Intermediate 3-2 (4.21 g) and TEA (2.0 g) in DCM (50 mL) was added benzoyl chloride (2.11 g) slowly. After stirring at room temperature for 1 hour and then the reaction was quenched with saturated sodium bicarbonate. The organic phase was dried over sodium sulfate and evaporated to dryness. Purification was achieved by chromatography on an ISCO column (RediSep 12, gradient elution with 10% to 70% EtOAc/Hex providing pure Intermediate 3-3 (2.82 g, 49% yield for the three steps).

후처리

  1. customthe reaction was quenched with saturated sodium bicarbonate
  2. dry with materialThe organic phase was dried over sodium sulfate
  3. customevaporated to dryness
  4. customPurification
  5. washRediSep 12, gradient elution with 10% to 70% EtOAc/Hex

출처 및 근거

ORD 기록
ord-f1da4701089a4d80a71528cdbe74b5fb
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08835422B2

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