Hydrochloric Acid → 6'-Bromospiro[cyclobutane-1,2'-inden]-1'(3'H)-imine

HRID 1770975

반응식

HRID 1770975 반응식
Cl.[Br:2][C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][CH:11]=1)[CH2:8][C:7]1([CH2:14][CH2:13][CH2:12]1)[C:6]2=[N:15]S(C(C)(C)C)=O.CCOCC>O1CCOCC1>[Br:2][C:3]1[CH:4]=[C:5]2[C:9]([CH2:8][C:7]3([CH2:14][CH2:13][CH2:12]3)[C:6]2=[NH:15])=[CH:10][CH:11]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 67979440N-(5'-Bromospiro[cyclobutane-1,2'-indene]-3'(1'H)-ylidene)-2-methylpropane-2-sulfinamide

생성물 1

HCID 679793936'-Bromospiro[cyclobutane-1,2'-inden]-1'(3'H)-imine

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

Hydrochloric acid (4M in 1,4-dioxane, 14.89 mL, 59.55 mmol) was added to a solution of N-(5′-bromospiro[cyclobutane-1,2′-indene]-3′(1′H)-ylidene)-2-methylpropane-2-sulfinamide (Example 54 Step 1, 2.11 g, 5.96 mmol) in anhydrous 1,4-dioxane (60 mL), and the resulting mixture was stirred under an argon atmosphere for 3 h. Et2O (4 mL) was added and the precipitate was filtered off and washed with Et2O, then partitioned between DCM (100 mL), and sat. aq. NaHCO3 (100 mL). The phases were separated and the organic layer concentrated to afford the title compound that was used as such without further purification.

후처리

  1. filtrationthe precipitate was filtered off
  2. washwashed with Et2O
  3. custompartitioned between DCM (100 mL), and sat. aq. NaHCO3 (100 mL)
  4. customThe phases were separated
  5. concentrationthe organic layer concentrated

출처 및 근거

ORD 기록
ord-f02e33a4102f4dd9b8542edceb107aa3
출처 데이터셋
uspto-grants-2016_02
특허 번호
US09248129B2

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