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Dichloromethane → HCID 44227675, 화합물

HRID 1441498
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HRID 1441498 반응식
[CH3:1][O:2][C:3]1[N:10]=[CH:9][CH:8]=[C:7]([CH3:11])[C:4]=1C=O.[C:12]([NH2:16])([CH3:15])([CH3:14])[CH3:13].[Cl-].[Ca+2].[Cl-].[CH2:20](Cl)Cl>>[C:12]([N:16]=[CH:20][C:8]1[CH:9]=[N:10][C:3]([O:2][CH3:1])=[CH:4][C:7]=1[CH3:11])([CH3:15])([CH3:14])[CH3:13]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 4

HCID 6344DichloromethaneHCID 6385Tert-ButylamineHCID 5284359Calcium ChlorideHCID 144935423-Pyridinecarboxaldehyde, 2-methoxy-4-methyl- (9CI)

생성물 1

HCID 44227675HCID 44227675, 화합물수율 89%

실험 절차

2-Methoxy-4-methylnicotinaldehyde (1.8 g, 12 mmol), tert-butylamine (15 mL), 3 Å molecular sieves (8 g) and dry DCM (10 mL) were mixed and allowed to stand at RT under protection from moisture (calcium chloride tube). After two days the mixture was filtered and the molecular sieves were washed several times with dry DCM. The combined washings were concentrated to give 2.2 g (89%) of the title compound as a crude oil that was used immediately in the next step.

후처리

  1. filtrationAfter two days the mixture was filtered
  2. washthe molecular sieves were washed several times with dry DCM
  3. concentrationThe combined washings were concentrated

출처 및 근거

ORD 기록
ord-d34addf32bd24ee798e6050a28bdc719
출처 데이터셋
uspto-grants-2010_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07655664B2

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