3-Methoxybenzylamine → 1,3-Di(3-Methoxybenzyl) Thiourea

HRID 1375749

반응식

HRID 1375749 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:10]=[CH:11][CH:12]=1)[CH2:6][N:7]=[C:8]=[S:9].[CH3:13][O:14][C:15]1[CH:16]=[C:17]([CH:20]=[CH:21][CH:22]=1)[CH2:18][NH2:19].COC1C=C(C=CC=1)CNC(N)=S>C(O)C>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:10]=[CH:11][CH:12]=1)[CH2:6][NH:7][C:8]([NH:19][CH2:18][C:17]1[CH:20]=[CH:21][CH:22]=[C:15]([O:14][CH3:13])[CH:16]=1)=[S:9]

참가 물질

5

반응물 3

HCID 211563-MethoxybenzylamineHCID 1265123-Methoxybenzyl isothiocyanateHCID 27595411-(3-Methoxybenzyl)-2-thiourea

생성물 1

HCID 102678421,3-Di(3-Methoxybenzyl) Thiourea

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
40 °C

실험 절차

The reaction of 3-methoxybenzyl isothiocyanate with 3-methoxybenzyl amine in ethanol was repeated doubling the reaction volume and reactants and heating for 2 h at 40° C. Crystallization at −10° C., followed by evaporation of the supernatant to 20 ml and a second crystallization gave 98.4% of the theoretical yield for the two crystallizations combined. Calculated elemental analysis of 3-methoxybenzyl thiourea: C, 64.53; H, 6.37; N, 8.85; S, 10.13. Found: C, 64.30; H, 6.46; N, 8.85; S, 10.09.

후처리

  1. customCrystallization at −10° C.
  2. customfollowed by evaporation of the supernatant to 20 ml
  3. customa second crystallization
  4. customgave 98.4% of the
  5. customtheoretical yield for the two crystallizations

출처 및 근거

ORD 기록
ord-55d71da4d1834758a3059e3f91977add
출처 데이터셋
uspto-grants-2007_01
특허 번호
US07169815B2

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