Bromine → HCID 20374951, 화합물

HRID 1448993

반응식

HRID 1448993 반응식
[Na].[CH2:2]([O:9][C:10]1[CH2:14][CH:13]([O:15][CH2:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH2:12][CH:11]=1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.BrBr.[CH3:25][NH:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH3:33]>C(O)CCCCCC.C1C=CC=CC=1>[CH2:27]([N:26]([CH3:25])[CH:12]1[CH:11]([O:9][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8])[CH:10]([O:9][CH2:2][C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH2:14][CH:13]1[O:15][CH2:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)[CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH3:33]

참가 물질

7

반응물 4

HCID 24408BromineHCID 93190N-MethylheptylamineHCID 5360545SodiumHCID 20374931HCID 20374931, 화합물

생성물 1

HCID 20374951HCID 20374951, 화합물

시약·촉매·용매 2

HCID 241Benzene용매2회HCID 8129Heptanol용매

실험 절차

0.23 g of sodium are dissolved in 30 ml of 1-heptanol at 50° under nitrogen. Dropwise, with stirring, there is added 4.88 g of N-heptyl-N-methyl-2-bromo-4,5-bibenzyloxycyclopentane-1-amine (obtainable from 3,5-dibenzyloxy-2-cyclopentene by the addition of bromine and reaction with 1-equivalent of methyl heptylamine), dissolved in 30 ml of benzene. Stirring is carried on for 6 hours at 50°. After cooling, 100 ml of benzene is added thereto. This is washed with water. The organic phase is dried over MgSO4 and the solvent is distilled off. After chromatographic purification of the residue (silica gel/chloroform:acetone=9:1), N-heptyl-N-methyl-5-heptyloxy-2,4-dibenzyloxy-cyclopentane-1-amine is obtained.

후처리

  1. stirringStirring
  2. customis carried on for 6 hours at 50°
  3. temperatureAfter cooling
  4. washThis is washed with water
  5. dry with materialThe organic phase is dried over MgSO4
  6. distillationthe solvent is distilled off
  7. customAfter chromatographic purification of the residue (silica gel/chloroform:acetone=9:1)

출처 및 근거

ORD 기록
ord-94ef12ff946346dc905bfdf4177f9e32
출처 데이터셋
uspto-grants-1980_02
특허 번호
US04188403

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