Hydrochloric Acid → HCID 69299496、化合物

HRID 2196500ノート

反応式

HRID 2196500 の反応式
[C:1]([C:3]1[S:7][CH:6]=[C:5]([N:8](C(OC(C)(C)C)=O)[NH:9]C(OC(C)(C)C)=O)[CH:4]=1)#[N:2].[ClH:24].O1CCOCC1>CC(O)C>[ClH:24].[NH:8]([C:5]1[CH:4]=[C:3]([C:1]#[N:2])[S:7][CH:6]=1)[NH2:9]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 59843278Di-tert-butyl 1-(5-cyanothiophen-3-yl)hydrazine-1,2-dicarboxylate

生成物 1

HCID 69299496HCID 69299496、化合物収率 97%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

To a stirring solution of compound 12 (1.38 g, 4.07 mmol) in 2-propanol (10 mL) was added 4M HCl in dioxane (10 mL, 40.0 mmol). The reaction heated to 80 degrees for 1 hour turning into a dark brown solution. The mixture was evaporated to dryness and the resulting the brown solid suspended and sonicated in diethyl ether. The suspension was filtered to afford compound 13 (0.701 g, 97%) as a brown solid. LRMS (ESI): calc. 139.0; found 140.1 (MH)+.

後処理

  1. temperatureThe reaction heated to 80 degrees for 1 hour
  2. customThe mixture was evaporated to dryness
  3. customsonicated in diethyl ether
  4. filtrationThe suspension was filtered

出典と根拠

ORDレコード
ord-7e624a66ce7e4c598f259738cf1ddbb4
出典データセット
uspto-grants-2012_12
特許番号
US08338437B2

反応ノート

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