Hydrochloric Acid → HCID 14234265, 화합물

HRID 1194756노트

반응식

HRID 1194756 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][S:9]([NH:12][CH2:13][C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)(=[O:11])=[O:10])=[CH:4][CH:3]=1.[N:20]([O-])=O.[Na+].[ClH:24]>O>[ClH:24].[NH:1]([C:2]1[CH:7]=[CH:6][C:5]([CH2:8][S:9]([NH:12][CH2:13][C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=2)(=[O:11])=[O:10])=[CH:4][CH:3]=1)[NH2:20]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 132861021-(4-Aminophenyl)-N-benzylmethanesulfonamideHCID 23668193Sodium Nitrite

생성물 1

HCID 14234265HCID 14234265, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A thick suspension of the product of stage (b) (3.68 g) in conc. hydrochloric acid (50 ml) was stirred at -5° whilst a solution of sodium nitrite (0.9 g) in water (10 ml) was added dropwise so that temperature did not exceed 0°. Stirring was continued for 30 min. The resulting suspension was filtered to remove starting material and the filtrate added in a few portions to a solution of stannous chloride dihydrate (13.5 g) in hydrochloric acid (15 ml) at -20° and warmed to ambient temperature. The solid that separated was filtered off and recrystallised from hot methanol (100 ml) to give the title compound as white plates (0.39 g) m.p. 192°-193°. The mother liquors afforded a second crop (0.52 g).

후처리

  1. additionwas added dropwise so that temperature
  2. customdid not exceed 0°
  3. filtrationThe resulting suspension was filtered
  4. customto remove
  5. additionthe filtrate added in a few portions to a solution of stannous chloride dihydrate (13.5 g) in hydrochloric acid (15 ml) at -20°
  6. customThe solid that separated
  7. filtrationwas filtered off
  8. customrecrystallised from hot methanol (100 ml)

출처 및 근거

ORD 기록
ord-c180ee72505c4f44b9b7aa32ef48f8e4
출처 데이터셋
uspto-grants-1989_03
특허 번호
US04816470

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