8-amino-5H-benzo[b][1,4]benzoxazepin-6-one → HCID 178465553, 화합물

HRID 895982노트

반응식

HRID 895982 반응식
[NH2:1][C:2]1[CH:3]=[CH:4][C:5]2[O:11][C:10]3[CH:12]=[CH:13][CH:14]=[CH:15][C:9]=3[NH:8][C:7](=[O:16])[C:6]=2[CH:17]=1.Br.C1C2C(=CC=CC=2)C=CC=1CS[C:31](=[NH:33])[CH3:32]>C(O)C>[O:16]=[C:7]1[C:6]2[CH:17]=[C:2]([NH:1][C:31](=[NH:33])[CH3:32])[CH:3]=[CH:4][C:5]=2[O:11][C:10]2[CH:12]=[CH:13][CH:14]=[CH:15][C:9]=2[NH:8]1

참가 물질

4

반응물 2

HCID 27563998-amino-5H-benzo[b][1,4]benzoxazepin-6-oneHCID 221387052-Naphthylmethyl ethanimidothioate hydrobromide

생성물 1

HCID 178465553HCID 178465553, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a stirred solution of 2-amino-10H-dibenzo[b,f][1,4]oxazepin-11-one (Example 4, 50 mg, 0.22 mmol) in 4 mL of ethanol at 0° C. was added thioacetimidic acid naphthalen-2-ylmethyl ester hydrobromide (65 mg, 0.22 mmol). The reaction was warmed to room temperature overnight. The mixture was concentrated at reduced pressure and partitioned between water (5 mL) and ethyl acetate (25 mL). The aqueous layer was separated and evaporated under vacuum (yield 70 mg, 92%). H1 NMR (DMSO d6) δ: 11.15 (bs, 1H), 10.68 (s, 1H), 9.44 (bs, 1H), 8.56 (bs, 1H), 7.71-7.70 (m, 1H), 7.54-7.53 (m, 2H), 7.40-7.36 (m, 1H), 7.20-7.17 (m, 3H), 2.31 (s, 3H), MS (ES): MH+ 268.3.

후처리

  1. concentrationThe mixture was concentrated at reduced pressure
  2. custompartitioned between water (5 mL) and ethyl acetate (25 mL)
  3. customThe aqueous layer was separated
  4. customevaporated under vacuum (yield 70 mg, 92%)

출처 및 근거

ORD 기록
ord-d1e932c3f07547b5934f1964769a7d45
출처 데이터셋
uspto-grants-2005_07
특허 번호
US06919328B1

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