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Diisobutylaluminumhydride → HCID 69737506, 화합물

HRID 2416535
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HRID 2416535 반응식
[H-].C([Al+]CC(C)C)C(C)C.C([O:13][C:14](=O)/[C:15](/[F:29])=[CH:16]/[C:17]1[CH:22]=[CH:21][C:20]([C:23]2[N:28]=[CH:27][CH:26]=[CH:25][N:24]=2)=[CH:19][CH:18]=1)C>C(Cl)Cl>[F:29]/[C:15](=[CH:16]\[C:17]1[CH:18]=[CH:19][C:20]([C:23]2[N:24]=[CH:25][CH:26]=[CH:27][N:28]=2)=[CH:21][CH:22]=1)/[CH2:14][OH:13]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 21225700DiisobutylaluminumhydrideHCID 69728829HCID 69728829, 화합물

생성물 1

HCID 69737506HCID 69737506, 화합물수율 98%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
0 °C

실험 절차

Diisobutylaluminum hydride (1.0 M solution in THF, 5.5 mL, 5.50 mmol) was added dropwise to a 0° C. solution of the product from step A (500 mg, 1.84 mmol) in methylene chloride (15 mL). The resulting solution was stirred for 10 min at 0° C., quenched with methanol (0.25 mL) followed by 15% aq. Rochelle salt (20 mL), and allowed to stir at room temperature for 4 h. The layers were separated and the aqueous layer was extracted with methylene chloride (20 mL). The combined organic layers were dried (MgSO4) and concentrated to provide 415 mg (98%) of the title compound as a colorless solid. MS 231 (M+H)+.

후처리

  1. customquenched with methanol (0.25 mL)
  2. stirringto stir at room temperature for 4 h
  3. customThe layers were separated
  4. extractionthe aqueous layer was extracted with methylene chloride (20 mL)
  5. dry with materialThe combined organic layers were dried (MgSO4)
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-fee6180ccbe04bf8ad3de45c2c46c686
출처 데이터셋
uspto-grants-2004_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06825170B2

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