C-(2,3-dihydro-benzo[1,4]dioxin-5-yl)-methyleneamine → 1-(2,3-Dihydro-benzo[1,4]dioxin-5-yl)-ethylamine

HRID 1988419

반응식

HRID 1988419 반응식
[O:1]1[C:6]2[CH:7]=[CH:8][CH:9]=[C:10]([CH:11]=[NH:12])[C:5]=2[O:4][CH2:3][CH2:2]1.[CH3:13][Mg]Br>C1(C)C=CC=CC=1.C(OCC)C>[O:1]1[C:6]2[CH:7]=[CH:8][CH:9]=[C:10]([CH:11]([NH2:12])[CH3:13])[C:5]=2[O:4][CH2:3][CH2:2]1

참가 물질

5

반응물 2

HCID 86618567C-(2,3-dihydro-benzo[1,4]dioxin-5-yl)-methyleneamineHCID 178418573HCID 178418573, 화합물

생성물 1

HCID 577255011-(2,3-Dihydro-benzo[1,4]dioxin-5-yl)-ethylamine

시약·촉매·용매 2

HCID 1140Toluene용매HCID 3283Diethyl Ether용매

반응 조건

온도
60 °C

실험 절차

The dried resin to which the C-(2,3-dihydro-benzo[1,4]dioxin-5-yl)-methyleneamine (1 eq) was bound was suspended in dry toluene. Under a nitrogen atmosphere methyl magnesium bromide (150 eq) in a 3 M solution in ethyl ether was added. This mixture was shaken for 24 hours at 60° C. then filtered and washed with toluene, water, then methanol and dichloromethane alternately three times. The final wash was with methanol. The solid was dried under vacuum.

후처리

  1. filtrationthen filtered
  2. washwashed with toluene, water
  3. washThe final wash
  4. customThe solid was dried under vacuum

출처 및 근거

ORD 기록
ord-52c249de9ebb4430914271b157d44391
출처 데이터셋
uspto-grants-2009_06
특허 번호
US07553854B2

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