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Carbonazidic acid, 1,1-dimethylethyl ester → HCID 178453124、化合物

HRID 1395784
ノート
印刷プレビュー

反応式

HRID 1395784 の反応式
Cl.[NH2:2][CH2:3][C:4]1[S:8][C:7]([SH:9])=[N:6][N:5]=1.[C:10]([O:14][C:15](N=[N+]=[N-])=[O:16])([CH3:13])([CH3:12])[CH3:11]>O.O1CCOCC1.C(N(CC)CC)C>[C:10]([O:14][C:15]([NH:2][CH2:3][C:4]1[S:8][C:7]([SH:9])=[N:6][N:5]=1)=[O:16])([CH3:13])([CH3:12])[CH3:11]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

HCID 61256Carbonazidic acid, 1,1-dimethylethyl esterHCID 178479189HCID 178479189、化合物

生成物 1

HCID 178453124HCID 178453124、化合物収率 65.2%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 8471Triethylamine溶媒HCID 312751,4-Dioxane溶媒2 回

実験手順

To a mixture of 5-aminomethyl-1,3,4-thiadiazole-2-thiol hydrochloride (5.5 g) in water (50 ml), dioxane (50 ml) and triethylamine (15 ml) was added t-butoxycarbonyl azide (5.6 g) and the mixture was stirred for 24 hours at 40° to 45° C. After the reaction was over, the dioxane was distilled off under reduced pressure. The residue was adjusted to pH2 with 10% hydrochloric acid and extracted twice with ethyl acetate. The extract was washed with a saturated aqueous solution of sodium chloride and then dried over magnesium sulfate and then evaporated to dryness to give 5-t-butoxycarbonylaminomethyl-1,3,4-thiadiazole-2-thiol (4.83 g). m.p. 144° to 146° C.

後処理

  1. distillationwas distilled off under reduced pressure
  2. extractionextracted twice with ethyl acetate
  3. washThe extract was washed with a saturated aqueous solution of sodium chloride
  4. dry with materialdried over magnesium sulfate
  5. customevaporated to dryness

出典と根拠

ORDレコード
ord-05b737cdbf65460c9f36137b9b700caa
出典データセット
uspto-grants-1980_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04205166

反応ノート

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