Dimethyl Sulfate → HCID 86633699, 화합물

HRID 502480노트

반응식

HRID 502480 반응식
[NH2:1][C:2]1[C:15]2[C:14](=[O:16])[C:13]3[C:8](=[C:9]([NH2:17])[CH:10]=[CH:11][CH:12]=3)[C:7](=[O:18])[C:6]=2[C:5]([O:19][CH2:20][CH2:21][N:22]([CH3:24])[CH3:23])=[CH:4][CH:3]=1.N[C:26]1C2C(=O)C3C(=C(N)C=CC=3)C(=O)C=2C(Cl)=CC=1.CNN(NC)CCO.[Na].[CH3:53][O:54][S:55]([O:58]C)(=[O:57])=[O:56]>O.ClC1C=CC=CC=1>[CH3:53][O:54][S:55]([O-:58])(=[O:57])=[O:56].[NH2:1][C:2]1[C:15]2[C:14](=[O:16])[C:13]3[C:8](=[C:9]([NH2:17])[CH:10]=[CH:11][CH:12]=3)[C:7](=[O:18])[C:6]=2[C:5]([O:19][CH2:20][CH2:21][N+:22]([CH3:26])([CH3:24])[CH3:23])=[CH:4][CH:3]=1

참가 물질

8

반응물 5

HCID 6497Dimethyl SulfateHCID 5360545SodiumHCID 204567661,5-Diamino-4-chloroanthracene-9,10-dioneHCID 22635088HCID 22635088, 화합물HCID 68702144HCID 68702144, 화합물

생성물 1

HCID 86633699HCID 86633699, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 7964Chlorobenzene용매

실험 절차

6.6 parts of 1,5-diamino-4-(2-dimethylamino-ethoxy)-anthraquinone prepared from 1,5-diamino-4-chloro-anthraquinone, N,N-dimethylaminoethanolamine and metallic sodium at 95-120° C. were dispersed in 75 parts of chlorobenzene and treated with 1.4 parts of dimethylsulfate. The reaction mixture was kept for 1½ hours at room temperature. The precipitate was filtered off and stirred with 150 parts of water followed by filtration. The filtrate was evaporated in vacuo yielding 2.5 parts of the dye of formula Ik. The red dye Ik is very good water-soluble. The analytic data are consistent with the assigned structure for dye Ik.

후처리

  1. waitThe reaction mixture was kept for 1½ hours at room temperature
  2. filtrationThe precipitate was filtered off
  3. filtrationfollowed by filtration
  4. customThe filtrate was evaporated in vacuo
  5. customyielding 2.5 parts of the dye of formula Ik

출처 및 근거

ORD 기록
ord-1e081e530a2740449be7d6ea7a70393f
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07776106B2

반응 노트

불러오는 중…