Hydrochloric Acid → HCID 86616004, 화합물

HRID 1987578노트

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HRID 1987578 반응식
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]

참가 물질

6

반응물 4

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

생성물 1

HCID 86616004HCID 86616004, 화합물수율 291.5%

시약·촉매·용매 1

HCID 962Water용매2회

반응 조건

온도
25 °C

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-54f1f3f8d62143288ddbbd602e2acee8
출처 데이터셋
uspto-grants-2009_06
특허 번호
US07550629B2

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