Dimethyl Sulfate → HCID 86633699、化合物

HRID 502480ノート

反応式

HRID 502480 の反応式
[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

参加物

8

反応物 5

HCID 6497Dimethyl SulfateHCID 5360545SodiumHCID 204567661,5-Diamino-4-chloroanthracene-9,10-dioneHCID 22635088HCID 22635088、化合物HCID 68702144HCID 68702144、化合物

生成物 1

HCID 86633699HCID 86633699、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 7964Chlorobenzene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1e081e530a2740449be7d6ea7a70393f
出典データセット
uspto-grants-2010_08
特許番号
US07776106B2

反応ノート

読み込み中…