Formaldehyde → 1-Acetamido-7-benzylmethylamino-5,6,7,8-tetrahydronaphthalene

HRID 863508노트

반응식

HRID 863508 반응식
[C:1]([NH:4][C:5]1[C:14]2[CH2:13][CH:12]([NH:15][CH2:16][C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)[CH2:11][CH2:10][C:9]=2[CH:8]=[CH:7][CH:6]=1)(=[O:3])[CH3:2].C=O.[C:25]([BH3-])#N.[Na+]>C(O)(=O)C>[C:1]([NH:4][C:5]1[C:14]2[CH2:13][CH:12]([NH:15][CH2:16][CH2:17][C:22]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:25]=3)[CH2:11][CH2:10][C:9]=2[CH:8]=[CH:7][CH:6]=1)(=[O:3])[CH3:2]

참가 물질

5

반응물 3

HCID 712FormaldehydeHCID 5003444Sodium cyanoborohydrideHCID 196961461-Acetamido-7-benzylamino-5,6,7,8-tetrahydronaphthalene

생성물 1

HCID 196962191-Acetamido-7-benzylmethylamino-5,6,7,8-tetrahydronaphthalene수율 103.8%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A mixture of 1-acetamido-7-benzylamino-5,6,7,8-tetrahydronaphthalene (14.3 g, 50 mmol), paraformaldehyde (15 g, 0.5 mol) and sodium cyanoborohydride (15.7 g, 0.25 mol) in acetic acid (250 mL) was stirred at room temperature for 48 h. The solvent was removed and the residue taken up in water:diethyl ether. The aqueous phase was basified with 12.5% NaOH and back extracted with ether. The combined ether layers were washed with saturated NaCl, dried over magnesium sulfate, filtered and evaporated to give a viscous syrup (16 g).

후처리

  1. customThe solvent was removed
  2. extractionback extracted with ether
  3. washThe combined ether layers were washed with saturated NaCl
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. customevaporated

출처 및 근거

ORD 기록
ord-ca1851245f03440facd11e8bc3793770
출처 데이터셋
uspto-grants-1998_02
특허 번호
US05721234

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