4-Methylpiperazine-1-ethylamine → 1-(6-Thiocyanato-1,3-benzothiazol-2-yl)-3-[2-(4-methylpiperazin-1-yl)ethyl]urea

HRID 633489

반응식

HRID 633489 반응식
[S:1]([C:4]1[CH:22]=[CH:21][C:7]2[N:8]=[C:9]([NH:11][C:12](=[O:20])OC3C=CC=CC=3)[S:10][C:6]=2[CH:5]=1)[C:2]#[N:3].[CH3:23][N:24]1[CH2:29][CH2:28][N:27]([CH2:30][CH2:31][NH2:32])[CH2:26][CH2:25]1>>[S:1]([C:4]1[CH:22]=[CH:21][C:7]2[N:8]=[C:9]([NH:11][C:12]([NH:32][CH2:31][CH2:30][N:27]3[CH2:28][CH2:29][N:24]([CH3:23])[CH2:25][CH2:26]3)=[O:20])[S:10][C:6]=2[CH:5]=1)[C:2]#[N:3]

참가 물질

3

반응물 2

HCID 702844-Methylpiperazine-1-ethylamineHCID 53472570Phenyl(6-thiocyanato-1,3-benzothiazol-2-yl)carbamate

생성물 1

HCID 866478811-(6-Thiocyanato-1,3-benzothiazol-2-yl)-3-[2-(4-methylpiperazin-1-yl)ethyl]urea

실험 절차

The 1-(6-thiocyanato-1,3-benzothiazol-2-yl)-3-[2-(4-methylpiperazin-1-yl)ethyl]urea was prepared according to the method described in Example 9c, but using 982 mg of phenyl (6-thiocyanato-1,3-benzothiazol-2-yl)carbamate and 473 mg of 2-(4-methylpiperazin-1-yl)ethylamine. The residue obtained is chromatographed on a Merck cartridge (25 g of silica 15-40 μm), elution being carried out with a 90/10 mixture of dichloromethane/methanol. 1.13 g of 1-(6-thiocyanato-1,3-benzothiazol-2-yl)-3-[2-(4-methylpiperazin-1-yl)ethyl]urea are thus recovered in the form of a white solid, the characteristics of which are as follows:

후처리

  1. customThe residue obtained
  2. customis chromatographed on a Merck cartridge (25 g of silica 15-40 μm), elution
  3. additionbeing carried out with a 90/10 mixture of dichloromethane/methanol
  4. custom1.13 g of 1-(6-thiocyanato-1,3-benzothiazol-2-yl)-3-[2-(4-methylpiperazin-1-yl)ethyl]urea are thus recovered in the form of a white solid

출처 및 근거

ORD 기록
ord-42d9d0cd55d84beba5b983a0aabd2ac1
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09321777B2

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