Hydrochloric Acid → HCID 86616004、化合物

HRID 1987578ノート

反応式

HRID 1987578 の反応式
N[C:2]1[CH:3]=[C:4]([S:9]([OH:12])(=[O:11])=[O:10])[CH:5]=[CH:6][C:7]=1[Cl:8].Cl.N([O-])=O.[Na+].[CH3:18][S:19]SC>O>[Cl:8][C:7]1[CH:6]=[CH:5][C:4]([S:9]([OH:12])(=[O:11])=[O:10])=[CH:3][C:2]=1[S:19][CH3:18]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 12232Dimethyl DisulfideHCID 668174-Chlorometanilic acidHCID 23668193Sodium Nitrite

生成物 1

HCID 86616004HCID 86616004、化合物収率 291.5%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

反応条件

温度
25 °C

実験手順

To a solution of 3-amino-4-chloro-benzenesulfonic acid (5.00 g, 24 mmol) in distilled water (38 mL) and concentrated HCl (6 mL, 72 mmol) at 0° C. was added sodium nitrite (1.99 g, 28.9 mmol) in H2O (10 mL). After 1.5 h, the mixture was allowed to warm to 25° C. and stirred for 1.5 h. Methyl disulfide (10.7 mL, 120 mmol) was added and the mixture heated to 70° C. for 18 h. The solvent was removed, in vacuo, to give an orange solid (16.7 g) that was used as is in the next reaction.

後処理

  1. temperaturethe mixture heated to 70° C. for 18 h
  2. customThe solvent was removed, in vacuo

出典と根拠

ORDレコード
ord-54f1f3f8d62143288ddbbd602e2acee8
出典データセット
uspto-grants-2009_06
特許番号
US07550629B2

反応ノート

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