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Diisobutylaluminum hydride → HCID 89556341, 화합물

HRID 578880
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HRID 578880 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[N:5]=[CH:4][C:3]=1[C:9]1([C:12]#[N:13])[CH2:11][CH2:10]1.CC(C[AlH]CC(C)C)C.[BH4-].[Na+].C(C(C(C([O-])=O)O)O)([O-])=O.[Na+].[K+]>C1(C)C=CC=CC=1.CO>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[N:5]=[CH:4][C:3]=1[C:9]1([CH2:12][NH2:13])[CH2:10][CH2:11]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

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HCID 14487Diisobutylaluminum hydrideHCID 4311764Sodium borohydrideHCID 9855836Potassium sodium tartarateHCID 89544502HCID 89544502, 화합물

생성물 1

HCID 89556341HCID 89556341, 화합물수율 97.2%

시약·촉매·용매 2

HCID 887Methanol용매
HCID 1140
Toluene
용매
2회

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온도
-10 °C

실험 절차

1-(4,6-Dichloro-3-pyridyl)cyclopropanecarbonitrile (0.1 g, 0.469 mmol) was dissolved in Toluene (2.3 mL). At −10° C. DIBAL-H 1M in Toluene (0.98564 mL, 0.986 mmol) was added dropwise. The reaction mixture was stirred 30 min at −10° C. At −10° C. NaBH4 (0.10871 g, 2.816 mmol) was added, then carefully 3 mL MeOH. The reaction mixture was stirred 30 min at rt. It was poured into 25 ml of 1N potassium sodium tartrate. The pale yellow solution was extracted 3 times with Ether. The combined organic phases were washed with brine and dried with Na2SO4, filtrated and the filtrate evaporated. The product was obtained as a pale yellow oil (99 mg).

후처리

  1. customAt −10° C
  2. customAt −10° C
  3. stirringThe reaction mixture was stirred 30 min at rt
  4. extractionThe pale yellow solution was extracted 3 times with Ether
  5. washThe combined organic phases were washed with brine
  6. dry with materialdried with Na2SO4
  7. filtrationfiltrated
  8. customthe filtrate evaporated

출처 및 근거

ORD 기록
ord-04d8bf1bce4d45f7b1e5d985f6d6de7d
출처 데이터셋
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09040708B2

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