Ammonium Hydroxide → HCID 13937644、化合物

HRID 2118430ノート

反応式

HRID 2118430 の反応式
[CH3:1][N:2]([S:4]([C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([C:13]([O:15][CH3:16])=[O:14])[C:8]=1[CH2:17][S:18](Cl)(=[O:20])=[O:19])(=[O:6])=[O:5])[CH3:3].[OH-].[NH4+:23]>O1CCCC1>[CH3:1][N:2]([S:4]([C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([C:13]([O:15][CH3:16])=[O:14])[C:8]=1[CH2:17][S:18]([NH2:23])(=[O:20])=[O:19])(=[O:6])=[O:5])[CH3:3]

参加物

4

反応物 2

HCID 14923Ammonium HydroxideHCID 14153224HCID 14153224、化合物

生成物 1

HCID 13937644HCID 13937644、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of the crude sulfonyl chloride from Example 13 in 150 ml of tetrahydrofuran was cooled to 0° and treated with 7.3 ml of concentrated aqueous ammonium hydroxide. The resulting suspension was allowed to warm to room temperature. Removal of the solvent in vacuo gave an oily residue which was triturated with 300 ml water. The precipitate was collected by filtration, washed with n-butyl chloride and dried to yield 9.3 g of 2-[(N,N-dimethylamino)sulfonyl]-6-(methoxycarbonyl)phenylmethanesulfonamide as a light yellow solid, m.p. 133°-142°; IR(nujol): 3400, 3310, 1720 cm-1 ; NMR (CDCl3 /DMSO-d6): δ 2.6 (6H, s, SO2N(CH3)2), 3.8 (3H, s, CO2CH3), 5.35 (2H, s, --CH2 --), 5.3-5.9 (2H, br s, NH2), 7.4-8.3 (3H, m).

後処理

  1. customRemoval of the solvent in vacuo
  2. customgave an oily residue which
  3. customwas triturated with 300 ml water
  4. filtrationThe precipitate was collected by filtration
  5. washwashed with n-butyl chloride
  6. customdried

出典と根拠

ORDレコード
ord-7fc1837ce14a4743b22b92cea2d30976
出典データセット
uspto-grants-1987_07
特許番号
US04678500

反応ノート

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